HRID747001

反应详情

EQUATION

反应方程式

HRID 747001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

(±) 3-(3-Bromo-4-fluorophenyl)-4-vinyltetrahydropyran-2-ol (from step f) above; 10.32 g, 0.034 mol), (1R)-3,5-bis(trifluoromethyl)phenylethanol (11 g, 0.042 mol), Amberlyst™ (5 g) and molecular sieves (8 g) were suspended in dichloromethane (20 mL) and the mixture was shaken at 40° C. for 3 days. The resulting yellow solution was filtered, concentrated in vacuo and was purified by chromatography on silica using 1-5% ethyl acetate in hexane as eluant to give a mixture of isomers 1-3 (which were retained) and the desired isomer 4 (3.6 g, 20%) as a colourless oil.

WORKUP

后处理

  1. filtrationThe resulting yellow solution was filtered
  2. concentrationconcentrated in vacuo
  3. customwas purified by chromatography on silica using 1-5% ethyl acetate in hexane as eluant
  4. customto give
  5. additiona mixture of isomers 1-3 (which were retained)