HRID1296548

反应详情

EQUATION

反应方程式

HRID 1296548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.00 g (17.1 mmol) 3-(2-Fluoro-4-trifluoromethyl-phenyl)-acrylamide, 2.60 g (21.3 mmol) 1,3-dichloroacetone and 40 ml toluene were kept at reflux temperature for 16 h with continuous removal of water by use of a Dean-Stark trap. After cooling to room temperature, two extractions with 100 ml water, the organic phase was dried over sodium sulphate and the solvent removed in vacuo. Chromatography on silica gel (eluent: n-heptane/ethyl acetate 5:1) gave 1.20 g (23%) 4-chloromethyl-2-[2-(2-fluoro-4-trifluoromethyl-phenyl)-vinyl]-oxazole.

WORKUP

后处理

  1. temperatureat reflux temperature for 16 h
  2. customwith continuous removal of water by use of a Dean-Stark trap
  3. extractiontwo extractions with 100 ml water
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. customthe solvent removed in vacuo