HRID1995509

反应详情

EQUATION

反应方程式

HRID 1995509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8.7 g (0.03 mol) of 6-iodoisatoic acid anhydride, 3.2 g (0.036 mol) of sarcosine and 25 ml of dimethylacetamide is heated to boiling under reflux for 1 hour. After cooling and dilution with water, the mixture is extracted with chloroform. The chloroform extracts are dried and evaporated. After recrystallization of the crude product from methylene chloride/ether, there is obtained 3,4-dihydro-6-iodo-4-methyl-2H-1,4-benzodiazepine-2,5(1H)-dione of melting point 214°-217°.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 1 hour
  3. temperatureAfter cooling
  4. extractiondilution with water, the mixture is extracted with chloroform
  5. dry with materialThe chloroform extracts are dried
  6. customevaporated
  7. customAfter recrystallization of the crude product from methylene chloride/ether