Nitric Acid → Ammonia

Participants

Reaction Steps

In a boiler of acid-resistant stainless steel of 800 liters capacity, provided with a stirring device, a cooling jacket and an efficient reflux condenser, 150 liters of nitric acid of 1.50 density preheated to about 85° was placed and stirred in order to maintain a constant temperature and a nitrated solution obtained as in example I was poured in dropwise and then 80 kg of 2-methylimidazole in 80 liters of concentrated sulphuric acid was added. The reacting solution was stirred until a clear diminishing of the exothermic effect was noted and the temperature was raised gradually, after 1 hour, to 110° and this temperature was maintained for 25 minutes. The reflux condenser was thereafter removed and the temperature increased to about 140° and was maintained at this level for 30-minutes, the volatile components being distilled off during that time and removed from the reacting medium. The reacted solution was cooled and divided, and 1/3 was left in the nitrator, and from the remaining 2/3 of this solution 2-methyl-5-nitroimidazole was isolated in known manner (by diluting with water and neutralizing with ammonia to pH about 6). 88 kg of product were obtained corresponding to about 77% of theoretical.

Provenance & Evidence