HRID33215

反应详情

EQUATION

反应方程式

HRID 33215 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 3-acetyl-7-chlorosulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine (4.0 g, 13.9 mmol), morpholine (1.8 ml, 20.8 mmol) and triethylamine (2.14 ml, 15.3 mmol) in tetrahydrofuran (120 ml) was heated at 60° C. for 3 h. The reaction mixture was then cooled, filtered and the filtrate evaporated in vacuo to give a yellow solid. Crystallisation from dichloromethane/n-hexane gave the title compound as an off-white solid (4.4 g, 94 Mass Spectrum AP+: Found 339 (MH+). C16H22N2SO4 requires 338.

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled
  2. filtrationfiltered
  3. customthe filtrate evaporated in vacuo
  4. customto give a yellow solid
  5. customCrystallisation from dichloromethane/n-hexane