HRID1763658
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
To 9-ethoxycarbonylamino-11-(3-dimethylaminopropylidene)-11H-pyrrolo[2,1-b][3]benzazepine (2.80 g.) in 100 ml. EtOH is added 10 ml. 2 N potassium hydroxide. Reflux is maintained for 42 hours. The volatiles are removed under vacuum and the residue is extracted with chloroform, washed with water, and dried over magnesium sulfate. Evaporation leaves a dark residue that is purified by chromatography on silica gel. Elution with 10% methanol in chloroform yields 9-amino-11-(3-dimethylaminopropylidene)-11H-pyrrolo[2,1-b][3]benzazepine.
WORKUP
后处理
- temperatureReflux
- temperatureis maintained for 42 hours
- customThe volatiles are removed under vacuum
- extractionthe residue is extracted with chloroform
- washwashed with water
- dry with materialdried over magnesium sulfate
- customEvaporation
- customleaves a dark residue that
- customis purified by chromatography on silica gel
- washElution with 10% methanol in chloroform