HRID444508

反应详情

EQUATION

反应方程式

HRID 444508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of carbon disulphide (8.36 g) in acetone (16 ml) was added dropwise to a stirred solution of 3-(3-aminopropoxy)-N,N-dimethylbenzenemethanamine (20.8 g) in acetone (60 ml) at -10° to 0° during 15 minutes. A solution of mercuric chloride (27.2 g) in acetone (40 ml) was added slowly at -15° and after the addition the suspension was warmed to 0° and triethylamine (23 g) added dropwise. The suspension was refluxed for 45 minutes then filtered and evaporated to give an oil which was chromatographed (alumina,grade 3/ether). The appropriate eluate was evaporated to a yellow oil consisting of the title compound (8.7 g).

WORKUP

后处理

  1. additionafter the addition the suspension
  2. temperaturewas warmed to 0°
  3. temperatureThe suspension was refluxed for 45 minutes
  4. filtrationthen filtered
  5. customevaporated
  6. customto give an oil which
  7. customwas chromatographed (alumina,grade 3/ether)
  8. customThe appropriate eluate was evaporated to a yellow oil