HRID223195

反应详情

EQUATION

反应方程式

HRID 223195 的结构方程式

PROCEDURE

实验过程

4.84 g (0.02 mol) of 6-bromoisatoic acid anhydride and 1.78 g (0.02 mol) of sarcosine are finely rubbed together and subsequently heated to 260° under a protective gas for 6 minutes. After cooling, the crude product is chromatographed on silica gel using chloroform/methanol (20:1) for the elution. After recrystallization from chloforom/hexane, there is obtained 6-bromo-3,4-dihydro-4-methyl-2H-1,4-benzodiazepine-2,5(1H)-dione of melting point 232°-233°.

WORKUP

后处理

  1. temperaturesubsequently heated to 260° under a protective gas for 6 minutes
  2. temperatureAfter cooling
  3. customthe crude product is chromatographed on silica gel
  4. washfor the elution
  5. customAfter recrystallization from chloforom/hexane