HRID223328
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
7.65 g (0.04 mol) of 6-ethylisatoic acid anhydride and 4.6 g (0.04 mol) of L-proline are suspended in 40 ml of dimethyl sulphoxide, heated to 70° for 2.5 hours, the solvent is removed in a high vacuum and the oil obtained is heated to 170° for 15 minutes. The crude product is purified by chromatography on silica gel using chloroform for the elution. There is obtained amorphous (S)-6-ethyl-1,2,3,11a-tetrahydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione.
WORKUP
后处理
- temperatureheated to 70° for 2.5 hours
- customthe solvent is removed in a high vacuum
- customthe oil obtained
- temperatureis heated to 170° for 15 minutes
- customThe crude product is purified by chromatography on silica gel
- washfor the elution