Edited From
http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0318 (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.
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)
(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_imgs/djvu.gif)
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