HRID1266149

反应详情

EQUATION

反应方程式

HRID 1266149 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(4-trichloroacetylpiperazin-1-yl) anisole (D1) (10 g) in dichloromethane (115 ml) was added over 0.3 h to ice-cooled chlorosulfonic acid (52 ml). After 0.5 h at 0° C. then 1 hour at ambient temperature, the solution was poured onto a mixture of ice-water (500 g) and dichloromethane (500 ml) with rapid stirring. The layers were separated and the organic phase was washed with water (2×800 ml), dried (MgSO4) and concentrated to give the title compound (D2) as a foam (6.0 g, 46%), MH+ 435/437.

WORKUP

后处理

  1. customThe layers were separated
  2. washthe organic phase was washed with water (2×800 ml)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated