HRID1449848

反应详情

EQUATION

反应方程式

HRID 1449848 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add methanesulfonic acid (47.7 kg, 496 mol) to a toluene solution of ethyl 2-(difluoromethyl)-2-(t-butoxycarbonyl)-4-(p-fluorophenyl)butyrate as prepared in Example 3.1 at a temperature of 40° C.-50° C. After 3 to 6 hours, cool the reaction to ambient temperature. Add toluene (91 kg) and water (421 kg) and stir for 30 minutes. Separate the aqueous layer. Add to the organic layer a 20% by weight solution of sodium chloride in water (420 kg) and stir for 30 minutes. Separate the layers to give the title compound as a solution in toluene.

WORKUP

后处理

  1. customas prepared in Example 3.1 at a temperature of 40° C.-50° C
  2. temperaturecool
  3. customthe reaction to ambient temperature
  4. customSeparate the aqueous layer
  5. additionAdd to the organic layer a 20% by weight solution of sodium chloride in water (420 kg)
  6. customSeparate the layers