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Topic created by Nitritespecialist
on Tue, 21 Jun 2022 at 17:41

Nitritespecialist said on Tue, 21 Jun 2022 at 17:41...

Org. Synth. 1936, 16, 7
DOI: 10.15227/orgsyn.016.0007
n-BUTYL NITRITE

Submitted by W. A. Noyes
Checked by C. R. Noller and B. H. Wilcoxon.

1. Procedure
In a 3-l. three-necked, round-bottomed flask, fitted with a mechanical stirrer (Note 1), a separatory funnel extending to the bottom of the flask, and a thermometer, are placed 380 g. (5.5 moles) of c.p. sodium nitrite and 1.5 l. of water. The flask is surrounded by an ice-salt mixture, and the solution is stirred until the temperature falls to 0. A mixture of 100 cc. of water, 136 cc. (250 g., 2.5 moles) of concentrated sulfuric acid (sp. gr. 1.84) (Note 2), and 457 cc. (370 g., 5 moles) of commercial n-butyl alcohol is cooled to 0 and by means of the separatory funnel is introduced slowly beneath the surface of the nitrite solution, with stirring. The alcohol solution is added slowly enough so that practically no gas is evolved, and the temperature is kept at 1. This usually requires from one and one-half to two hours.

The resulting mixture is allowed to stand in the ice-salt bath until it separates into layers, and the liquid layers are decanted from the sodium sulfate into a separatory funnel (Note 3). The lower aqueous layer is removed and the butyl nitrite layer washed twice with 50-cc. portions of a solution containing 2 g. of sodium bicarbonate and 25 g. of sodium chloride in 100 cc. of water. After drying over 20 g. of anhydrous sodium sulfate, the yield of practically pure butyl nitrite amounts to 420440 g. (8185 per cent of the theoretical amount) (Note 4) and (Note 5). If desired, the product may be distilled under reduced pressure when 98 per cent distils at 2427/43 mm. (Note 6). Butyl nitrite boils at 75 under atmospheric pressure, with some decomposition.

2. Notes
1. A stirrer capable of keeping solid material in motion and driven by a strong motor should be used because of the precipitation of large amounts of sodium sulfate towards the end of the reaction.
2. The concentration of sulfuric acid which is used keeps the butyl alcohol in solution but does not dissolve butyl nitrite.
3. If more butyl nitrite separates from the sodium sulfate after the first decantation, a second decantation is made. Care must be exercised in handling butyl nitrite; inhalation of the vapor may cause severe headache and heart excitation.

4. The same procedure is quite satisfactory for runs of one-tenth this size. In small runs mechanical stirring is unnecessary since gentle rotation of the flask by hand gives good mixing.

5. Isoamyl nitrite may be made in the same manner and with approximately the same yields.
6. Butyl nitrite decomposes slowly on standing and should be kept in a cool place and used within a few days or, at most, a few weeks after it is prepared. A sample which stood for five months during a warm summer seemed to contain only 2025 per cent of the original nitrite. The products of decomposition consist of oxides of nitrogen, water, butyl alcohol, and polymerization products of butyraldehyde.
Working with Hazardous Chemicals
The procedures in Organic Syntheses are intended for use only by persons with proper training in experimental organic chemistry. All hazardous materials should be handled using the standard procedures for work with chemicals described in references such as "Prudent Practices in the Laboratory" (The National Academies Press, Washington, D.C.,

BrewMeister... said on Tue, 21 Jun 2022 at 17:46...

May I draw your attention to No. 4.

William Noyes, the published chemist who wrote this procedure in 1936, says all that is necessary to do smaller brews is gentle HAND swirling of the contents. 1/10th of the brew size here is about 45 mls of alcohol.

You don't need a mechanical stir bar strong enough to plow through sodium sulfate crystals. Just shake and swirl during the addition of the acid. And add little bits of water after the reaction is all done...to aid separation of the ester from the sulfate crystals.

Popperasswipe said on Tue, 21 Jun 2022 at 18:04...

Hey everyone....when I made my poppers, I didn't so no blue. Was my brew a bust?

PopperExpert said on Tue, 21 Jun 2022 at 18:07...

@Popperass....not necessarily. Any blue nitrous acid shouldn't hang around for long. The sulfuric acid, low water method I used didn't turn blue at all and I got great poppers.

The Professor said on Wed, 22 Jun 2022 at 23:32...

Ken's still playing with his imaginary friends

everything they are saying now has been debunked years ago, but at this new site, which can't ban anybody, he's flipped out, screwed his own integrity, and somehow thinks he's teaching ME a lesson?

readers that are new to this forum probably haven't experienced the lying, deceitful, willful ignorance that is Ken (aka anonymous, aka popperass, aka madeplentypoppers, aka NitriteSpecialist aka PopperExpert, aka PopperMaker, aka kenjoneslee, aka John Mulligan, etc.

He'll fight his wrong ideas to the ground, hasn't attained control of this reaction 13 years, and is wasting everyone's time.

another big yawn with no new content, a dollop of lies, with a dash of baloney

Those interested in the REAL science can always refer to the wiki, and join PopperMakers (a subreddit) if you need support for it.)

wiki:
https://nublu.maitriworks.org/files/Alky%20Nitrite%20Preparation%20wiki.pdf

Maker's forum:

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