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  #41  
Old 09-08-2009, 11:27 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

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Originally Posted by 2bfrank View Post
Yeah, I agree the use of paraformaldehyde should work,theires also the possibility to make the dianion and then alkylate, but that would be troublesome, less OTC etc.
Not entirely sure what you mean here. Would you mind explaining?
Quote:
Id like to look at this via microwaves.
Haha, yes! Wouldn't we all?
Quote:
experiments to be done
Indeed. Will you be posting the results here or on vespiary?
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If you hvnt checked out that site I gave, do so, as its got some really good chem books..2bfrank.
I've seen it, most of the books look really interesting, but again, time prevents me from checking them out.
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Old 09-08-2009, 01:53 PM
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Default Re: OTC Mescaline Synthesis from Vanillin

Just read what I wrote and deleted and wrote this instead, the mechanism that you questioned about, uses a lithium base, 2M excess, and creates an enolate. The base results in overal removing 2 protons alpha to nitrogen forming the heteroenolate, being N(+) , a double bond between nitrogen and alpha carbon, alpha carbon being charged(2e's)and both oxygens being charged. Then on one oxygen this charge resonates and creates a carbonyl, which moves the double bond between the nitrogen and the alpha carbon, and those electrons move to the alpha carbon, = 4e's where 2 of them can attack say a methyl iodide. Thats more accurate, than what I wrote.. I cant find the paper, and this is from scribbly notes and memory.. Its sort of interesting, but requires say n-butylliithium, or something of that nature..not imposible but CHOH seems better

Results will be here, considering our discussions. Im currently making clayfen, FeNO3, CuNO3, and will load silicon gel, bentonite, and perhaps invest in some other types of clay.

Ha and yes, small world.. I thought you were refering to something when you said, it was nice seeing Frank in the smaller forums.. I haven't been posting for long full stop.
Blown out, somewhat, by how many people are into experimental chemistry.<..>
Got to go. 2b

ps, checked my files and found quite a bit on microwave henry condensations

Last edited by 2bfrank; 09-08-2009 at 02:37 PM.
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Old 09-08-2009, 03:17 PM
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Default Re: OTC Mescaline Synthesis from Vanillin

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Originally Posted by 2bfrank View Post

ps, checked my files and found quite a bit on microwave henry condensations
Post them please, i would love them!
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Old 09-09-2009, 12:26 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

I cannot see a link, to upload files to a message?? I can copy some but.

Microwave-Assisted Henry Reaction:
Solventless Synthesis of Conjugated Nitroalkenes
Tetrahedron Letters, Vol. 38, No. 29, pp. 5131-5134, 1997
Abstract: In a solventless system and under microwave irradiation, nitroaikanes react with
arylaldehydes in the presence of a catalytic amount of ammonium acetate to afford, in one step,
conjugated nitroalkenes without the isolation of intermediary ~-nitro alcohols.
1997 Elsevier Science Ltd.

The condensation of aldehyde with nitroalkanes using a catalytic amount of ammonium acetate (0.25
mmol/mmol of carbonyl compound used) coupled with the pulsed microwave irradiation is found to be an ideal condition that affords high yields of the conjugated nitroalkenes directly without the isolation
of the intermediary 1,3-nitroalcohols. That the effect is not purely thermal 25 is supported by the
fact that using an alternate heating mode (oil bath) at the same temperature of 90 C, the reaction
(c~-naphthaldehyde, entry 8j) could be completed in 18 hours
.
In a typical synthetic procedure, a mixture of benzaldehyde 5a (0.106 g, 1 retool) and nitromethane 6a
(0.061 g, 1 mmol) is placed in glass tube containing ammonium acetate (0.019 g, 0.25 retool) and is exposed to pulsed microwave irradiation 28 in an alumina bath for 2 min using an unmodified microwave oven operating at its 40% power. 25 The reaction mixture is cooled to room temperature (~ 1 min) and is irradiated again for 2 min. After two such successive irradiations (2 min) and cooling (~ 1 min) sequences, another 1 mmol of nitromethane is added to the reaction mixture that is further irradiated for two similar successions. After completion of the reaction (followed by TLC), the reaction mixture is passed through a short silica gel column using hexane:AcOEt (9:1,v/v) as an eluent. The evaporation of the solvent on a rotary evaporator affords beta-nitrostyrene (8a). Other nitroalkenes prepared following this general procedure are summarized in the Table.

In conclusion, we have developed an environmentally benign method for the rapid synthesis of
conjugated nitroalkenes that avoids the use of excessive nitrohydrocarbons and proceeds in
high yields.
yields are on a table, that for straight benz is around 80%, but I am sure their are better papers, that report better yields, I bit rushed.

and one for styrene.

Selective Nitration of Styrenes with Clayfen and Ciayan:
A Solvent-free Synthesis of beta-Nitrostyrenes
Tetrahedron Letters 39 (1998) 3977-3980

General procedure for the conversion of styrene to beta-nitrostyrene: In a typical experiment, styrene (180 mg,
1.74 mmol) was admixed with clayfen or clayan (300 mg) in a glass tube. The reaction mixture was placed in an
oil bath for 15 min or irradiated for 3 min in an alumina bath inside an unmodified household microwave oven
(900 watt) at its medium power. On completion of the reaction, followed by TLC examination (hexane:EtOAc,
4:1, v/v), the product was extracted into dichloromethane (45 mL), the combined organic extract dried with
anhydrous sodium sulfate and solvent removed under reduced pressure.

Reaction conditions: for clayfen, either in oil bath (15 min) or in microwave, MW. (3 min) at 100-I 10 *C and for clayan, either in
oil bath (15 min) or in MW (3 rnin) at 60-70 "C.
their is a fair few preps of this around I beleive, and clayfen, clayan, claycop etc, are on Rhodium.

Dont know about anyone else, but Ill be testing the Al2O3 bath, aprox 5cm diameter, for temp over time. Pulsed and straight.

pss @nshanin, also the formation of a dianion, something I am sure you know and understand, and it was just my lack of the lingo, etc, was possibly overkill, but the more acidic, the less nucleophilic, hence was of interest.I also may of got it all wrong, I am not a chemist, learning etc. I do know when it comes to nitroalcohols the lithium gets involved-more than just stabalizing charge,This link has some old bits and some newer bits on the usefulness of this. http://www.unc.edu/depts/mtcgroup/li...s/dianions.pdf

Last edited by 2bfrank; 09-09-2009 at 05:09 AM.
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  #45  
Old 09-13-2009, 12:59 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

Soz to double up, but reduction also via Microwave, so the only step perhaps that is not, is the seclective reduction of the beta-nitrostyrene.. Even this may well be done in the bun. see http://www.rsc.org/delivery/_Article...m?doi=a808223e for scope
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Old 09-13-2009, 02:49 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

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Soz to double up, but reduction also via Microwave, so the only step perhaps that is not, is the seclective reduction of the beta-nitrostyrene.. Even this may well be done in the bun. see http://www.rsc.org/delivery/_Article...m?doi=a808223e for scope
Dammit I love Asian authors, always coming up with the newest and best techniques for us clandestine chemists. Not like typical US chemists doing TSes of massive products with limited applicability.
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Old 09-13-2009, 05:47 AM
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Yeah, but I tell you, if many of us etc, had 100% access to analytical instruments, with motivation that many do fucking have..lol's then man, wed be cutting edge for sure..and not sure about the reduction, as to unowot, but it may well be...Fuck, total nightmare if its doable for the big boy players.. WHAT they aren't buying much this week, and WHAT microwave oven sales have reached an all time HIGH. WTF....hahahahah.

hows the claycop,, toluene > the honey from his eyes..I wonder if scaling up is that greater issue. OH well. I cant see a problem with 100 vials,, lol;s worst case scenario 100X7 or was it 2Osecs..whaaat a fucking drag......

one more thing I found, and that is brewery supply benotonite can easily be used and turned into K-10 I think its called, via refluxing in acidic solution..theirs a fair bit of stuff on this, patents what not. There's also stuff about doing this with FeCl3 and its use in Friedel-Crafts alkylation. Now that would be something.. Bit of an issue with diaryl products, but pretty convinced that this can work for lots of reactions via loaded clay. and of course its entirely theoretical, for the novelty apect.. and the abitiy to do some interesting chem

Last edited by 2bfrank; 09-14-2009 at 09:18 AM. Reason: coz I can
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Old 09-13-2009, 07:47 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

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one more thing I found, and that is brewery supply benotonite can easily be used and turned into K-10 I think its called, via refluxing in acidic solution..


I thought I was the only who saw the immense value in K-10! This is great to hear.

Quote:
theirs a fair bit of stuff on this, patents what not. There's also stuff about doing this with FeCl3 and its use in Friedel-Crafts alkylation. Now that would be something.. Bit of an issue with diaryl products, but pretty convinced that this can work for arylketones, via loaded clay.
Yeah, F-Cs with activated clays are fantastic, especially their high yields and ability to use the straight acids or esters. Also, the clay itself is Bronsted acidic, and you know what that means...
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Old 09-13-2009, 08:59 AM
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"Also, the clay itself is Bronsted acidic, and you know what that means" mind giving me a hand in understanding this some more ... I thought a bronsted acid, was proton donating, and I assumed that the loading of say FeCl3, and I really haven't looked at the surface structure of clays, silicates, and how these ions would interact(and SHould/shall), but I thought the Fe+ associated with the clay surface, would be acting somewhat as a lewis acid and he accepting say a Cl- from an alkyl halide and act typicaly as in the F-Cls now youve thrown in the bronsted word, and also the use of straight acids, or esters.. I am trying to see their relationship with F-C's. mind giving me some understanding with this...

and of course this is all theoretical. I am pretty sure I have been clear on this..

just came back to this, and thought about this a little, and very briefly read these clays have pockets, somewhat like anion holes in enzymes, which may be lined with Fe(3+) ions, and themselves act as electron acceptors, and then I found this,, somewhat exciting as one can play around with these formations.. VOTC...and yeah yeah ammonia acetate/amine aint no drama, but thought i'd post this find, as finding this, I feel that catalysts for many purposes can be made..

Preparation of the Mg-Al hydrotalcite (3:1) catalyst:
Two separate solutions namely solution A containing Mg(NO3)2.6H2O (115.38 g, 0.45 mole)
and Al(NO3)3.9H2O (56.27 g, 0.15 mole ) in 300 ml of distilled water and solution B cotaining
NaOH (30 g) and Na2CO3 (15 g) in 200 ml of distilled water were prepared at room temperature.
Both solutions A and B were added simultaneously through a burette to a 1 L beaker containing 300
ml of distilled water at room temperature. The rate of addition of metal nitrates was maintained at
about 60 ml/h., while the pH of the reaction mixture was maintained alkaline by adjusting the flow
rate of solution B. After completion of addition of solution A, the resulting slurry was digested at 65
oC for 30 min. with constant stirring. The resulting precipitate was washed with distilled water
several times until the pH of the filtrate was 7.0. The catalyst was then dried at 100 oC and calcined
at 450 oC respectively for 8 h in air. The other ratios of the above catalyst, Mg-Al 4.0, 5.0 were
prepared by following the above procedures similarly, other catalysts, Zn-Al 3.0 and Cu-Al 3.0,
were prepared using Zn(NO3)2 and Cu(NO3)2 respectively.
General procedure for the preparation of 2-nitroalcohols:
A solution of substituted benzaldehyde(or plain benzaldehyde) (2 mmol), nitroalkane (2 mmol) and Mg-Al-HT (3:1)
(100 mg, 20%w/w) in THF (10 ml) was refluxed under nitrogen atmosphere for 6 h. The progress of
the reaction was monitored by TLC (10% EtOAc in pet ether), the catalyst was filtered off and the
product purified by flash chromatography (6% EtOAc in pet-ether as eluent) to afford nitropropan-1-
ol (41-95%). Spectral data for entries 1, 2, 5, 6, 9 and 12 studied for the predominant threo
selectivity given are for the mixtures of diastereomers. That is 3:1 dextro v levo..

Plug in Mg-Al hydrotalcite and see the scope in this, the ease,, I dare say 2b's the slow one with this,

"I thought I was the only who saw the immense value in K-10" was that a serious comment or a hint at my slowness, for if its true, then Fuck,,who ever is reading this, check the scope on this shit..ITS somewhat biggly

Last edited by 2bfrank; 09-14-2009 at 03:14 AM.
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Old 09-14-2009, 03:46 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

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"Also, the clay itself is Bronsted acidic, and you know what that means" mind giving me a hand in understanding this some more ... I thought a bronsted acid, was proton donating, and I assumed that the loading of say FeCl3, and I really haven't looked at the surface structure of clays, silicates, and how these ions would interact(and SHould/shall), but I thought the Fe+ associated with the clay surface, would be acting somewhat as a lewis acid and he accepting say a Cl- from an alkyl halide and act typicaly as in the F-Cls
K-10 is both Bronsted and Lewis acidic...
Quote:
Originally Posted by An Excllent Paper on the Subject
Most of the chemical reactions occurring on montmorillonites are based on the acidic properties (Bronsted and Lewis acidity) of their surfaces [4].
The Bronsted acidity is generated by the exchangeable cations, which, upon
their polarizing action, enhance the dissociation of the interlayer water
molecules. Partial dehydration increases the acidity. Natural montmorillonites
have surface acidities, as measured by the Hammett Ho acidity function, ranging from 1.5 to 3. Washing the clay with mineral acid, i.e.
exchanging the interlamellar Na+, K+, etc. cations with protons, brings their
surface acidity to He values between -5.6 to -8 [5].
Quote:
now youve thrown in the bronsted word, and also the use of straight acids, or esters.. I am trying to see their relationship with F-C's. mind giving me some understanding with this...
Well the problem with F-Cs in clandestine synthesis is that they require acid chlorides, which aren't the easiest thing to make. Thus there has been research into using straight acids or esters, like this patent. Now of course I'm not trying to imply that using K-10 is as effective as using TsOH or MeSO3H (free papers are out there), but Bronsted acidity clearly helps F-Cs along.

That wasn't my main point with the Bronsted comment though. Think about this: Most clandestine reactions focus on a way to get an amine onto a molecule. What if you could just combine two molecules (one of them being an amine) through some sort of reaction (an F-C perhaps) and make the amine from that. Naturally, amines don't work in F-C reactions because they're too nucleophillic and attack the acyl species immediately (and sadly, most work has gone into looking for protecting groups for these amines as a way to tone down their nucleophilicity), but assuming we use some sort of carboxylic acid with an amine functionality (call it an "amino acid" although it doesn't need to be an alpha-AA) then there will be no amines in the reaction mixture--only ammonium ions. At pH -3 there's no way any amine will exist as a freebase, thus preventing the acyl species from being attacked. Now we all know F-Cs form ketones, and with the above, we could potentially form amines too. So now we have a viable path towards amino ketones.

Now of course, all of the above discussion is useless for clandestine chemists because I've never heard of an abusable drug that has a benzyllic ketone group.

Naturally, the "amino acid" that you use in the F-C may potentially be N-methylated (or protected somehow if desired acidity is not reached and not enough clay is used--obviously for any of this to work you'll need a shitload of excess protons) in order to prevent imine formation or perhaps just for the hell of it.

But that doesn't matter because the clandestine community isn't hard at work thinking of ways to N-methylate amino acids (you, frank, have expressed a particular disinterest in the topic). And even if the above was possible, we all know there are no drugs of abuse with an N-methyl group. Pfffft.

Quote:
ammonia acetate/amine aint no drama
You're right, so let's leave it at that. Besides, NH4OAc gets you to the alkene whereas this procedure stops at the alcohol.
, but thought i'd post this find, as finding this, I feel that catalysts for many purposes can be made..

Quote:
Plug in Mg-Al hydrotalcite and see the scope in this, the ease,, I dare say 2b's the slow one with this,
Also just found this, its fucking free, downloadable etc.http://www.jstage.jst.go.jp/browse/bcsj/68/1/_contents
These mother fuckers get up to some wicked fucking shit,, and they share, not like all these other Fucks, So cation exchange I think is what I initialy missed..
I can't see it. I've been looking for a few J. Chem. Soc. Jpn. articles for a while now, if you can see them for free...

Quote:
was that a serious comment or a hint at my slowness, for if its true, then Fuck,,who ever is reading this, check the scope on this shit..ITS somewhat biggly
Serious comment; not many underground people are 'sperimentin' with it AFAIK. It's fucking huge. Oh, btw, google "deep eutectic solvents". Just like clay is the clandestine zeolite, those are the clandestine ionic liquid.
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Old 09-14-2009, 04:21 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

Just quickly, as I want to read all that you've stated in more detail, but the Bull chem, well I plugged in K-10, and lucked out with a freebie, I then mentioned it to someone other, and they returned with a NOPE< i then thought I edited that comment, swore I did, but will have to now, their appears to be a link of availabilities and I must of reached that with my first search, hence thought they were all free, some are, but dam it, they are interesting preps I have found. very cool and interesting uses of things, so Ill dam well pay for the privilege if I have to, and ill share what I can..

and thanks big time,, trying to get my head around the things stated,,will get their but will take some time..sort of like that when hit with things unfamiliar..so app'ted,

Last edited by 2bfrank; 09-14-2009 at 04:28 AM.
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Old 09-14-2009, 07:50 AM
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"That wasn't my main point with the Bronsted comment though. Think about this: Most clandestine reactions focus on a way to get an amine onto a molecule. What if you could just combine two molecules (one of them being an amine) through some sort of reaction (an F-C perhaps) and make the amine from that. Naturally, amines don't work in F-C reactions because they're too nucleophillic and attack the acyl species immediately (and sadly, most work has gone into looking for protecting groups for these amines as a way to tone down their nucleophilicity), but assuming we use some sort of carboxylic acid with an amine functionality (call it an "amino acid" although it doesn't need to be an alpha-AA) then there will be no amines in the reaction mixture--only ammonium ions. At pH -3 there's no way any amine will exist as a freebase, thus preventing the acyl species from being attacked. Now we all know F-Cs form ketones, and with the above, we could potentially form amines too. So now we have a viable path towards amino ketones."

for starters, i see I think where your going with the use of say a super acid, that protonates and forms a weak, but possible leaving group, that leaves and stays left, due to DStrap, So the next points,
you going alanine, perhaps protected,,with unsubstituted/substituted B. Or somehow the use of benzoic...perhaps reacting with a substituted alkene, or is my noobish glowing in the dark here..OH well.
My lack of amino protection interest, isn't due to anything other than the novelty of what we've discussed, got nothing much against doing what we have discussed to an amine, and perhaps that would of followed somewhat.
It may well be that I am misunderstanding,but wouldn't the amine group have to remain in the alpha position, alpha to the carboxy turned OH. Anyway, it is interesting, and I will give this some more thought...

What would be good, if this amine would not need to be protected, other than being protonated, without it turning into an SN2 situation, due to acidic solution, so it would want to be really acidic, and not allow any neuclophile to exist to react... possible do you reckon,, perhaps a shitload of clay as mentioned, as well as an (i just edited a dumbass possibility lol's)

.

Last edited by 2bfrank; 09-14-2009 at 08:55 AM.
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Old 09-14-2009, 09:29 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

No you're completely misunderstanding me. Let me spell it out for you:



...with pictures.
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Old 09-14-2009, 10:17 AM
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I did state "you going alanine, perhaps protected,,with unsubstituted/substituted B." B as in benzene, perhaps you thought I meant the benzaldehyde, but I didn't and would say if I did,,I knew by your description that One carboxylic acid with either B for benzene, and then I through in the possibility of going benzoic, and somehow reacting that with an alkene,(substituted somehow with an amine) and really wasn't clear, so the picture has sorted this out and thanks.I hadn't thought of this, other than piecing some of this together from your description of your novel prep.. It is VERY very interesting, Not just for the target depicted, not by a long shot..OH yeah, YOU WERE 100% correctomundo, about the selective reduction of beta-nitrostyrene... got shown a paper today..a local mob too.. Details if you want..

So THeirs no possibility of not protecting the amino group, and purely relying on the lone pair being protonated,, doubtful ha.. I say this purely in light of problematic work up heard regarding forming the N-methylalanine. I keep looking at this picture, INTERESTING INDEED...

actualy work up for the N-methylation of the aa could surely be tweeked, as it uses a buffer system to keep things not to acidic, If one was really thoughtful about this, one may not have to extract the aa ect..

Last edited by 2bfrank; 09-14-2009 at 10:33 AM.
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Old 09-14-2009, 11:04 AM
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Details if you want..

Please be more specific in your abbreviations. "B." means nothing to me, neither does "benzoic" if it's outside of the proper context (as it was in what you said).

Quote:
So THeirs no possibility of not protecting the amino group, and purely relying on the lone pair being protonated,, doubtful ha.. I say this purely in light of problematic work up heard regarding forming the N-methylalanine. I keep looking at this picture, INTERESTING INDEED...
Honestly? Amines will be protonated in this media regardless of how they're substituted (I mean shit, look at the mechanism for superacid-catalyzed F-Cs, you protonate a fucking carbonyl!). There's no possibility for imine formation (and the subsequent Pictet-Spengler reaction, which is one of the major threats here) when your amine can't attack an electrophile. Any discussion about protection was purely theoretical and in all likelihood irrelevant. Besides, if this reaction really fucks up you'll need way more than ONE methyl group on your amine to salvage it.

Quote:
actualy work up for the N-methylation of the aa could surely be tweeked, as it uses a buffer system to keep things not to acidic, If one was really thoughtful about this, one may not have to extract the aa ect..
My thoughts exactly.
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Old 09-14-2009, 11:17 AM
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Can we get post 48 and on moved to a different thread, maybe title it "The wonderful world of clay!"
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Old 09-14-2009, 11:31 AM
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Yes in total agreement, and dare I say MORE< but at some point in time it'll be good to discuss "deep eutectic solvents" with respect to chemheads being somewhat forced to do things hard...

and seeing abstracts such as >>> Acidities up to 10^12 times that of sulfuric acid have now been obtained. The extremely low nucleophilicity of the counterions in superacidic systems is especially useful for the preparation of stable, electron-deficient cations, particularly carbocations. Many of these cations, which were formerly detectable only in the gas phase, can now be studied in solution. Novel organic syntheses that are not possible in ordinary acidic media can also be achieved in superacids, including syntheses of economically important hydrocarbons. The unique ability of superacids to bring about hydrocarbon transformations, even to activate methane to undergo electrophilic oligocondensation, can open up new fields in chemistry.

looking very very interesting indeed..

Last edited by 2bfrank; 09-15-2009 at 03:13 AM.
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Old 09-23-2009, 06:38 AM
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nshanin, in the paper you found that promoted the acyl cation via a super acid system, hence the possibility to use an amino acid etc, what pH or pKa value did the paper report in using..or could you give me the name of the paper or aurthors of said..if pos. thanks.
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Old 09-23-2009, 07:52 AM
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nshanin, in the paper you found that promoted the acyl cation via a super acid system, hence the possibility to use an amino acid etc, what pH or pKa value did the paper report in using
Anhydrous TsOH. Also, Dean-Stark.

Quote:
..or could you give me the name of the paper or aurthors of said..if pos. thanks.
http://www3.interscience.wiley.com/j...TRY=1&SRETRY=0

Look her up. I'm tellin' you, man, these Asian authors
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Old 09-23-2009, 09:18 AM
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Ahh yes, just the paper I needed to see.. Dam no access, YET and that old catch phrase - just a matter of time Mr Carboxy - has just been turned into, please stay, your more than welcome Mr C, but whilst your hanging around, mind helping out somewhat hahahah, yes, so things are looking mighty fine indeed..Still, whist I wait for the total paper viewing, if you do have it handy, pKa??or Ho relative to H2SO4, which appears to be standard measurment of superacids..Oh well, best I be patient, its not as if Mr C is going places..well not in this context..just helping out and changed.


Actually I got the prep, but not the yield via SM but not for what were considering/your take on its potential.... Interesting that the possibility that youve presented has not been discussed..Perhaps the novelty. I will still find out the pH of this system, as their may be easier ways, more OTC, to get their...but then again TsOH, allthough not being done by I, it does not look that difficult.

Last edited by 2bfrank; 09-23-2009 at 10:46 AM.
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Old 09-25-2009, 04:26 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

Full paper:
http://www.mediafire.com/?ozmjhmdmzt5

Refs 8a and 8b look interesting but in fact use the acyl halides.

More on zeolites (I sadly don't have access): http://www.rsc.org/publishing/journa...i=c39950002307

Deep eutectic solvents are interesting because there are dozens of novel applications for ionic liquids, one of the more interesting ones being the use of carboxylic acids for the selective acylation of (substituted) indoles at the 3 position.

Last edited by nshanin; 09-25-2009 at 04:32 AM.
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Old 09-25-2009, 11:00 PM
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Default Re: OTC Mescaline Synthesis from Vanillin

Just saw this, thanks,, best I get my files in myshareware sorted, as I got a couple that touch on this,, will have a go at sorting this out today..
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Old 09-28-2009, 12:16 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

Quote:
Originally Posted by nshanin View Post
Full paper:
http://www.mediafire.com/?ozmjhmdmzt5

Refs 8a and 8b look interesting but in fact use the acyl halides.

More on zeolites (I sadly don't have access): http://www.rsc.org/publishing/journa...i=c39950002307

Deep eutectic solvents are interesting because there are dozens of novel applications for ionic liquids, one of the more interesting ones being the use of carboxylic acids for the selective acylation of (substituted) indoles at the 3 position.
the article in question plus one more on F-C's

http://www.4shared.com/file/13587031..._Catalyst.html
http://www.4shared.com/file/13587045...catalysts.html
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Old 10-04-2009, 02:00 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

I thought I was the only one who saw value in K-10 ha, NOW THAT IS AN UNDERSTATEMENT>.
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Old 10-10-2009, 06:57 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

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Originally Posted by Fractals View Post
Damn, I though it would be easy when wikipedia said "the simplest being the esterification of sulfuric acid with methanol."
Simplest/Deadliest.

DMS is batshit dangerous; It's nearly 4 times more poisonous than cyanides.
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Last edited by Leshrac; 10-10-2009 at 07:00 AM. Reason: spellzing :P
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Old 10-19-2009, 01:29 AM
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Default Re: OTC Mescaline Synthesis from Vanillin

Quote:
Originally Posted by Leshrac View Post
Simplest/Deadliest.

DMS is batshit dangerous; It's nearly 4 times more poisonous than cyanides.
Not really. All you need to do is what you should have already if your working with chemicals: a fume hood/glove box, disposable nitrile gloves and goggles.

If you use an airtight glove box with thick lab gloves there is virtually no exposure to it and it's not dangerous at all.

The only real problem is disposing of it safely w/o initiating chemical warfare with waste management.

and;

Quote:
Originally Posted by 2bfrank View Post
So THeirs no possibility of not protecting the amino group, and purely relying on the lone pair being protonated,, doubtful ha.. I say this purely in light of problematic work up heard regarding forming the N-methylalanine. I keep looking at this picture, INTERESTING INDEED...

actualy work up for the N-methylation of the aa could surely be tweeked, as it uses a buffer system to keep things not to acidic, If one was really thoughtful about this, one may not have to extract the aa ect..
fmoc protection ftw!!

Last edited by pooter; 10-19-2009 at 01:43 AM.
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Old 10-19-2009, 07:38 PM
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Originally Posted by pooter View Post
The only real problem is disposing of it safely w/o initiating chemical warfare with waste management.
Lmao.
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