HRID1763658

反应详情

EQUATION

反应方程式

HRID 1763658 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureReflux
  2. temperatureis maintained for 42 hours
  3. customThe volatiles are removed under vacuum
  4. extractionthe residue is extracted with chloroform
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. customEvaporation
  8. customleaves a dark residue that
  9. customis purified by chromatography on silica gel
  10. washElution with 10% methanol in chloroform