HRID1039678

反应详情

EQUATION

反应方程式

HRID 1039678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A solution of 1,1,1-trifluoro-2-(4-methoxyphenyl)propan-2-ol (22.5 g, 102 mmol) in 150 ml of anhydrous toluene was treated sequentially with pyridine (8.26 ml, 102 mmol) and dropwise sulfuryl dichloride (11.2 ml, 153 mmol) at 0° C. The resulting mixture was then heated at 55° C. for 18 h. The reaction was diluted with 100 ml of EtOAc, washed with 100 ml of H2O and 100 ml of 1N HCl, dried over Na2SO4, and concentrated to give an oil which was filtered through a silca gel pad eluting with 0-5% EtOAc in hexanes to afford the title compound.

WORKUP

后处理

  1. washwashed with 100 ml of H2O and 100 ml of 1N HCl
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customto give an oil which
  5. filtrationwas filtered through a silca gel pad
  6. washeluting with 0-5% EtOAc in hexanes