HRID223333

反应详情

EQUATION

反应方程式

HRID 223333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.3 g (0.015 mol) of 6-chloro-5-fluoroisatoic acid anhydride and 2 g (0.017 mol) of L-proline in 7.5 ml of dimethylformamide are heated to 120° for 2 hours, cooled, treated with 12 ml of distilled water and the precipitated brown crystals are filtered off. By recrystallization of the crude product from acetone/hexane there is obtained (S)-6-chloro-7-fluoro-1,2,3,11a-tetrahydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione of melting point 217°-219°.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationthe precipitated brown crystals are filtered off
  3. customBy recrystallization of the crude product from acetone/hexane there