HRID2190304

反应详情

EQUATION

反应方程式

HRID 2190304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 3,3-bis(4-fluorophenyl)propan-1-ol (4.99 g, 20.1 mmol) in pyridine (60 mL) at 0° C. was added 4-methylbenzene-1-sulfonyl chloride (4.20 g, 22.0 mmol). The reaction mixture was stirred at 0° C. for 4 h, warmed to room temperature and stirred for 4 h. The reaction mixture was partially concentrated, diluted with EtOAc, washed with 1 M HCl (2×), saturated NaHCO3 (1×), brine (1×), dried over MgSO4, filtered, and concentrated to give 3,3-bis(4-fluorophenyl)propyl 4-methylbenzenesulfonate which was used in the next step without further purification.

WORKUP

后处理

  1. temperaturewarmed to room temperature
  2. stirringstirred for 4 h
  3. concentrationThe reaction mixture was partially concentrated
  4. additiondiluted with EtOAc
  5. washwashed with 1 M HCl (2×), saturated NaHCO3 (1×), brine (1×)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated