HRID1937000
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
A solution of 1,2,3,3a,5,9b-hexahydrocyclopenta[c]quinolin-4-one (374 mg, 2.0 mmol) in DMF (10 ml) is mixed with N-bromosuccinimide (356 mg, 2.0 mmol). After 15 minutes of stirring at room temperature, the batch is heated for 15 minutes to 100° C., diluted with water and extracted with methyl-tert-butyl ether. The combined extracts are dried (Na2SO4) and concentrated by evaporation in a vacuum. The residue is purified on silica gel with ethyl acetate-hexane: 470 mg (88%) of product.
WORKUP
后处理
- temperaturethe batch is heated for 15 minutes to 100° C.
- extractionextracted with methyl-tert-butyl ether
- dry with materialThe combined extracts are dried (Na2SO4)
- concentrationconcentrated by evaporation in a vacuum
- customThe residue is purified on silica gel with ethyl acetate-hexane