HRID1936581

反应详情

EQUATION

反应方程式

HRID 1936581 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 668 mg of 2,3-diamino-6-nitrotoluene, 20 mL of glacial acetic acid and 2 mL of 12N hydrochloric acid is heated to reflux for 3 hours. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with 20 mL of water, and basified with ammonium hydroxide (28-30%). The resulting suspension is extracted with ethyl acetate and the extracts are dried over magnesium sulfate, filtered and rotary evaporated to provide 720 mg of 2,4-dimethyl-5-nitrobenzimidazole as a tan solid.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux for 3 hours
  3. extractionThe resulting suspension is extracted with ethyl acetate
  4. dry with materialthe extracts are dried over magnesium sulfate
  5. filtrationfiltered
  6. customrotary evaporated