HRID973302

反应详情

EQUATION

反应方程式

HRID 973302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-diethylaminoethanol (814 mg.) and pyridine (10 ml.) is added at 0° C. to 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride (3.07 g.). The mixture is stirred at room temperature until the acid chloride dissolves, and the solution is stored at 0° C. for 2 days. The mixture is filtered and the filtrate evaporated. The residue is triturated with ether and combined with the solid previously filtered off. The combined solids are crystallised from dioxan-ether to give 2-diethylaminoethyl 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionate hydrochloride (2.2 g.), m.p. 139°-140° C. (decomposition).

WORKUP

后处理

  1. dissolutiondissolves
  2. filtrationThe mixture is filtered
  3. customthe filtrate evaporated
  4. customThe residue is triturated with ether
  5. filtrationpreviously filtered off
  6. customThe combined solids are crystallised from dioxan-ether