HRID1154454

反应详情

EQUATION

反应方程式

HRID 1154454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13.0 g (128.4 mmol) of L-azetidine-2-carboxylic acid and 22.7 g (128.4 mmol) of 6-methyl-isatoic acid anhydride in 150 ml of dimethyl sulphoxide are heated to 95° for 3 hours, evaporated to dryness in a high vacuum and the residue obtained is heated to 140° for 2.25 hours. By crystallization from ethyl acetate there is obtained (S)-1,10a-dihydro-5-methyl-2H-azeto[2,1-c][1,4]benzodiazepine-4,10(9H)-dione of melting point 159°-160°.

WORKUP

后处理

  1. customevaporated to dryness in a high vacuum
  2. customthe residue obtained
  3. temperatureis heated to 140° for 2.25 hours
  4. customBy crystallization from ethyl acetate