Nitric Acid → 2-Methyl-5-nitroimidazole

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.

1. dissolutionwas dissolved
2. additionwith simultaneous mixing
3. temperaturecooling
4. additionwas gradually added so that
5. temperaturecooling
6. temperaturea constant temperature of 80° was maintained
7. addition15 minutes after addition of all the reagents
8. temperaturea gradual increase of temperature, 10° in each 15 minutes
9. customwas noted until a temperature of 110°
10. temperatureThe solution was maintained at that temperature for 20 minutes
11. temperaturethe temperature of the reacting mixture increased to about 140°
12. distillationwhereby the volatile components were distilled from the reaction medium
13. wait1/4 of the solution was left for treatment in a similar way for the
14. additionfollowing charge and from the remaining 3/4 of the solution

ORD record

ord-d87893b007814cd481e4c0f2d75f27c2

Source dataset

uspto-grants-1980_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04209631