Nitric Acid → 2-Methyl-5-nitroimidazole

Participants

Reaction Steps

In a nitrated solution obtained as in example VIII 75 kg of 2-methylimidazole was dissolved with simultaneous mixing and cooling. The reflux condenser was connected and 120 liters of nitric acid of 1.50 density poured in, whereafter sulphuric acid was gradually added so that by simultaneous stirring and cooling, a constant temperature of 80° was maintained. 15 minutes after addition of all the reagents, a gradual increase of temperature, 10° in each 15 minutes, was noted until a temperature of 110° was reached. The solution was maintained at that temperature for 20 minutes and thereafter the reflux condenser was disconnected and the temperature of the reacting mixture increased to about 140°, whereby the volatile components were distilled from the reaction medium. 1/4 of the solution was left for treatment in a similar way for the following charge and from the remaining 3/4 of the solution there were isolated, in known manner, 98 kg of 2-methyl-5-nitroimidazole corresponding to about 70% of theoretical.

Provenance & Evidence