HRID33204

反应详情

EQUATION

反应方程式

HRID 33204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-acetyl-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine (1.75 g, 6.55 mmol) in 5 M hydrochloric acid was heated at reflux for 18 h. The reaction mixture was then cooled to room temperature, basified to pH=12 with potassium carbonate and the solvent evaporated in vacuo. The solid residue was then extracted with ethyl acetate (5×60 ml) and the combined organics dried (Na2SO4). The solvent was then evaporated in vacuo to give the title compound (450 mg, 32%) as a pale yellow oil.

WORKUP

后处理

  1. temperatureat reflux for 18 h
  2. customthe solvent evaporated in vacuo
  3. extractionThe solid residue was then extracted with ethyl acetate (5×60 ml)
  4. dry with materialthe combined organics dried (Na2SO4)
  5. customThe solvent was then evaporated in vacuo