HRID35067

反应详情

EQUATION

反应方程式

HRID 35067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-14 °C

PROCEDURE

实验过程

A solution of carbon disulphide (3.3 ml) in acetone (8 ml) was added dropwise to a solution of 3-[3-(1-piperidinylmethyl)phenoxy propanamine (12.4 g) in acetone (30 ml) over a 15 minute period, between -5° and -10° C. The solution was cooled to -14° C. and mercury (II) chloride (13.6 g) in acetone (30 ml) was added, during 45 minutes. Triethylamine (16 ml) was added at 0° C. during 15 minutes, and the mixture was heated at reflux for 45 minutes. The resulting suspension was purified by filtration and the filtrate evaporated in vacuo. The residue was purified by column chromatography using methanol as eluant to give the title compound (6 g) as an amber oil.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 45 minutes
  3. filtrationThe resulting suspension was purified by filtration
  4. customthe filtrate evaporated in vacuo
  5. customThe residue was purified by column chromatography