HRID1736454

反应详情

EQUATION

反应方程式

HRID 1736454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,3-diamino-6-nitrotoluene (11.81 g), formic acid (88%, 390 mL) and 12N HCl (38 mL) is heated to reflux for 1 hour. The resulting mixture is cooled to room temperature and rotary evaporated. The residue is diluted with water (200 mL), then basified with ammonium hydroxide (28-30%). The suspension is extracted with ethyl acetate (3×200 mL). The combined extracts are dried over magnesium sulfate (MgSO4) and evaporated to afford 4-methyl-5-nitrobenzimidazole as an orange solid.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux for 1 hour
  3. extractionThe suspension is extracted with ethyl acetate (3×200 mL)
  4. dry with materialThe combined extracts are dried over magnesium sulfate (MgSO4)
  5. customevaporated