Zoklet.net - Flasks and Beakers

HNO3(dilute) to make NO2

Anders Hoveland — Sat, 18 May 2013 06:17:26 GMT

This is not a drug thread, but for any you connoisseurs of chemistry out there, you may find this lab preparation interesting.

It is both indirectly inferred several places in the chemical literature that nitric oxide can selectively reduce dilute nitric acid to nitrogen dioxide. The reaction is:

(2)HNO3 + NO --> (3)NO2 + H2O

other related and better know equilibrium are:
(2)NO2 + H2O <==> HNO2 + HNO3
(2)HNO2 <==> H2O + NO + NO2

Here is some research I found:

Quote:

"Unlike reduction of nitrite to nitric oxide and of hydroxylamine to ammonium, which have mid point potentials of +300mV and +800mV, respectively"

the redox potential of the nitric oxide/ nitrite couple is Em>7 = +374 mV (Wood, 1978),

My question is: Is there any other common reducing agent besides nitric oxide that could be used to reduce dilute nitric acid to nitrogen dioxide, but not any further?

I know nitrogen dioxide can also be made from moderately concentrated nitric acid on copper, but it would be much more convenient is 5% nitric acid, for example, could be used instead.

You may be wondering what real advantage there would be, since it is well know that nitrogen dioxide can be easily prepared from the reaction of moderately concentrated nitric acid on copper metal.

(3)Cu + (8)HNO3 --> (3)Cu[NO3]2 + (2)NO + (4)H2O

(2)NO + O2 --> (2)NO2

If the nitric acid is between a concentration of around 20 to 30%, nitric oxide gas will be produced, which then spontaneously reacts with air to form the brown colored nitrogen dioxide. If 60% nitric acid concentration is used, then nitrogen dioxide is produced directly out of solution. There seems to be no observable reaction, however, when 4% concentrated nitric acid is used with copper, even after several days. Even the reaction with 20% nitric acid is somewhat inconveniently slow.

Consider, in the reaction between moderately concentrated nitric acid and copper, that 4 molar equivalents of 30% nitric acid are required to produce each molar equivalent of nitric oxide.

By subsequently passing this [one molar equivalent] of nitric oxide into a separate dilute solution of nitric acid, three molar equivalents of nitrogen dioxide can be obtained. And here lies the great advantage. For if the nitric oxide was simply allowed to react with air, only a single molar equivalent of nitrogen dioxide would be obtained.

It should be noted that the nitric oxide must react with the nitric acid in a separate reaction container, which does not contain copper metal. The precise reason for this implies substancially higher NO2 solubility, further reaction with the copper, and a complex state of equilibrium. Suffice to say that the NO2 reaction rate with copper is significantly faster than its reaction with moderately concentrated HNO3, since the action of HNO3 on copper must rely on the slight equilibrium formation of nitronium ions, NO2[+].

Cu + (4)NO2 --> Cu(NO3)2 + (2)NO

(3)HNO3 <==> NO2[+] + H3O[+] + (2)NO3[-]

If >60% concentrated nitric acid is used, reacting with copper to directly produce nitrogen dioxide straight out of solution, the efficiency can be relatively improved. Consider that in the reaction using concentrated nitric acid to produce nitrogen dioxide, two molar equivalents of nitric acid are required to produce each equivalent of nitrogen dioxide.

Cu + (4)HNO3 --> Cu(NO3)2 + (2)H2O + (2)NO2

If it is desired to produce nitrogen dioxide, the reaction of only moderately concentrated nitric acid with copper, and then the subsequent passing of the resulting nitric oxide gas into a separate solution of dilute nitric acid, will result in much less waste. Comparing the net required reactants to production of nitrogen dioxide, it can be seen that the last alternative is as efficient in its consumption of nitric acid as the use of concentrated nitric acid, although 3 times as much copper is wasted.

procedure reacting NO with air, Net Cost:
(3)Cu and (8)HNO3 ==> (2)NO2

procedure directly producing NO2, Net Cost:
(1)Cu and (4)HNO3 ==> (2)NO2

procedure reacting NO with additional separate HNO3, Net Cost:
(3)Cu and (12)HNO3 ==> (6)NO2

Thus if the availability of concentrated nitric acid is much more inconvenient than the availability of moderately concentrated nitric acid, or even of moderately concentrated sulfuric since a nitrate salt could be added with the same effect, it may likely be more desirable to utilize the special procedure described in this post.

MDMA SYNTHESIS

jordan119911 — Fri, 17 May 2013 22:19:43 GMT

Could someone with good knowledge tell me if this mdma synth i found online is legit

150 litres of MDP2P is added to 400 litres of N-methylformamide, the mixture was left stirring for 60 minutes and in the meantime 75 litres of 85% formic acid was added. The solution was heated to 190C (water and formic acid will distill off at 140C), no vacuum distillation was required, after the receiver flask presents ammonia smell the heating was stopped and the solution left to cool. 350 litres of H2O were added to remove excess N-methylformamide, separate 160 litres of the oil layer and extract the residual oil with 2x 30 litres dichloromethane or Et2O, distill the solvent out at 60C and 200hg. Add 180 litres of the oil to 100 litres of methanol, 250 litres 30% HCl in 550 litres H2O was added mixed and temperature raised to 65C to distill the MeOH over, after all of the MeOH was distilled off the solution was heated to 95C and left there for 3 hours. The solution was cooled, washed with 40 litres dichloromethane and decanted, the water layer was basified with 100 kilos of NaOH in 100 litres H2O, do NOT exceed the 40C when adding the base, at pH 10.3 100 litres of MDMA freebase will separate, this was extracted with 3x 30 litres dichloromethane, the extracts dried over MgSO4. The dichloromethane was distilled off. The pure MDMA base was dissolved into 300 litres dry acetone and gassed with HCl. Recrystallization was done from acetonitrile/IPA. Yield: 116 kilo MDMA.HCl

^^^^^^^^^^^^
This is a yield of 116 kilo, idealy id wanna make about a kilo

Any input would be sweet :D

De-fat iso poppy extraction

scottlee — Thu, 16 May 2013 20:13:07 GMT

Ive read that toluene is used to de-fat a simple water based poppy pod extraction. If someone wanted to perform the extraction using isopropyl alcohol insead of wated as it evaporates faster what could used instead of toluene, I belive it is miscible in isoproply. Ive read about melting paraffin wax and mixing it till it solidifys then filtering it out in a water based tek. Will this work for an alcohol based one?

Hydromorphone from Codeine

beaker — Tue, 07 May 2013 20:00:35 GMT

In a 50 ml rbf add 1.5part codeine,.47 p sulfuric acid, 9.8p water and .3p 10percent pd on c
Reflux for about 45min, filter hot
Base with koh 30 percent and extract into xylene with several small portions
To the xylene in a flask add 2parts k metabisulfite in water conc and stir vigorously for one hour put in fridge overnite
Filter xtls of adduct suspend in water add naoh to liberate the alkaloid
Dry for hydrocodone base hyperpure yeild 50 to 60percent much higher if skip bisulfite.

Dissolve hc base in 48 hbr acid and add 2 parts borax add another 5parts acid. Reflux for 6hours goes a violet color and base with ammonnia extract with chloroform evap for hm.
Yeild is v good.

Qualitatively the product was good but needed more or better demethylatiin maybe 12hrs

Can I get some halp please (DMT Extraction)

litefire — Sat, 04 May 2013 21:13:05 GMT

So a friend of a friend finally managed to get a source for MHRB (Fuck YOU DEA) and ordered 2 kilo's of bark. He told me that he has made DMT several times before, all with varying sucess. You see, he's not a chemist, the highest level of chemistry he has is Basic Chemistry in College. That being said, he and I both feel like something is seriously wrong if he cannot pull off a simple DMT extraction, right?

So here's the process he's been using:

250g MHRB was added to a glass jar. Around the same amount of NaOH was mixed with enough dH2O to cover the bark. This was added to the bark after it was allowed to cool down a bit.
I'm assumed this is where he's fucking up. Seems like way too much lye, right? But it took about that amount to get to PH 13, which is what he and I have both read is about what you want the PH at. Also, I remember reading a guide by Bunghole or someone else that said an almost equal ratio of MHRB:NaOH is optimal. :confused:

Anyways, this was allowed to sit for a few days, stirring everyday several times a day. After about 3 days, he added 200mL warm naptha and waited an hour or two then pulled the naptha, and put the naptha in the freezer. I remember he used to get huge amounts of white crystals on the first, second and third pull, but now he's getting MAYBE 60mg PER PULL, and it's really dirty yellow-brown.

He ended up doing maybe 6 pulls on each extraction and he's left with under a gram of DMT. What the fuck?? Any help would be greatly appreciated..:whistle:

bromocriptine questions

cws910 — Fri, 03 May 2013 20:09:05 GMT

So there's our lovely little molecule. Its unscheduled and unwatched, mainly because everyone figures that little bromine will stick around or somehow muck up a reaction...

#1. would the basic conditions used to hydrolyze the compound catalyze a dehalogenation (base catalyzed decomposition)? I read on some EPA site that temps in excess of 600deg F are used, but could that be countered by expanding the length of the reaction?

#2. Glycolate Dehalogenation. From the looks of it, once again, the hydrolysis and dehalogenation could be done at once (wouldn't the glycol actually speed up the hydrolysis?)

Extracting drugs from urine

ebdi — Fri, 03 May 2013 04:11:58 GMT

Some drugs pass through uncovered in substantial quantities. Ive heard up to 75% for some amphetamines but I have no source on that. What could somebody do to extract drugs from urine? Obviously purely theoretical, I doubt id ever be in a position to want to attempt.