Edited From

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0318

Hydroxylamine hydrochloride can be prepared technically  the action of sodium bisulfite on sodium nitrite. Raschig, who discovered the latter process, suggested the use of calcium nitrite and bisulfite so that the bulk of the inorganic salts could be removed in the form of calcium sulfate. Excellent yields have been reported by the reaction of acetone and sodium nitrite with zinc dust.

This seems like an amazingly easy OTC route to Hydroxylamine.hcl and also does not use nitromethane.

Does anyone know of a good write up or yields? Also how best to extract the Hydroxylamine.hcl. No quantities were given at orgsyn.com.

Sodium Nitrate can be bought by the bag as fertilizer. Unfortunately Calcium Nitrate fertilizer is a mix of ammonium, calcium and magnesium nitrates. Sodium bisulfate at can be bought at brew shops and spa supply shops as a ph reducer.

You need nitr_i_te not nitr_a_te.

Does anyone know of a good write up or yields? Also how best to extract the Hydroxylamine.hcl. No quantities were given at orgsyn.com.
A writeup better than that in Organic Syntheses?! You must not have closely read the Org. Syn. procedure; it gives, as always, complete details.

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Baseline Does Not Exist.

Doing too much research and not reading everything quite so clearly.  The info is there, though a way to do this without sulfur dioxide and without ether would be much prefferable.

The write up also does not cover the excellent yields have been reported by the reaction of acetone and sodium nitrite with zinc dust, though it is mentioned.

>Sodium Nitrate can be bought by the bag as fertilizer. Unfortunately Calcium
>Nitrate fertilizer is a mix of ammonium, calcium and magnesium nitrates. Sodium bisulfate

Ok. It's sodium bisulfite and sodium nitrite! It appears to me the workup involves producing acetone ketoxime to purify it, a very simple procedure. Also, the volumes are really large. Are you sure you can't buy a hydroxylamine salt at a photography store?

I also firmly believe they will get much harder in the next year.  This is why purely otc routes need to be worked out.

Raschig wasn't the only one that published the synthesis of hydrdoxylamine from a sulfite and a nitrite, Divers and Hata published several papers as well    The article's citations are JCS 659 (1886) and 1610 (1896)

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