HRID1154633

反应详情

EQUATION

反应方程式

HRID 1154633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.8 gm of glacial acetic acid in 10 ml of dioxane was added dropwise to a suspension of 1.3 gm (6 mmols) of 7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one and 1.1 gm (3 mmols) of sodium borohydride in 20 ml of dioxane; the mixture was refluxed for 3 hours, concentrated by evaporation and mixed with water. The mixture was extracted twice by shaking with methylene chloride; the extract was concentrated by evaporation, and the residue was taken up in ether. After filtering, the ether was removed in vacuo.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 3 hours
  2. concentrationconcentrated by evaporation
  3. additionmixed with water
  4. extractionThe mixture was extracted twice
  5. concentrationthe extract was concentrated by evaporation
  6. filtrationAfter filtering
  7. customthe ether was removed in vacuo