HRID544426

反应详情

EQUATION

反应方程式

HRID 544426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of 1.26 g of (1R,3R) 2,2-dimethyl-3-(2,2-dibromoethenyl)-cyclopropane-carboxylic acid chloride in 8 ml of benzene was added with stirring at 5° C. to a solution of 0.8 g of (2-benzyl-5-thiazolyl)-methanol in 8 ml of benzene and 0.8 ml of pyridine and the mixture was stirred at 20° C. for 17 hours and was poured into aqueous 2N hydrochloric acid solution with stirring. The decanted organic phase was washed with water and evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and eluted with a 7-3 hexane-ethyl acetate mixture to obtain 1.41 g of (2-benzyl-5-thiazolyl)-methyl (1R,3R) 2,2-dimethyl-3-[2,2-dibromoethenyl]-cyclopropane-1-carboxylate melting at 66° C. and having a specific rotation of [α]D20 =+9°±1° (c=1% in benzene).

WORKUP

后处理

  1. stirringwith stirring
  2. washThe decanted organic phase was washed with water
  3. customevaporated to dryness under reduced pressure
  4. customThe residue was chromatographed over silica gel
  5. washeluted with a 7-3 hexane-ethyl acetate mixture