HRID483748

反应详情

EQUATION

反应方程式

HRID 483748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (RS)-1,1,1-trifluoro-2-(4-ethoxyphenyl)propan-3-ol (0.4 g), 3-phenoxybenzyl bromide (0.45 g), tetra-n-butyl-ammonium hydrogen sulphate (0.05 g) and aqueous sodium hydroxide solution (40% w/v, 5.0 cm3) was stirred at the ambient temperature for 6 hours after which it was partitioned between water and diethyl ether. The ethereal phase was separated, washed twice with water, dried over anhydrous magnesium sulphate and concentrated by evaporation of the solvent under reduced pressure. The residual oil (0.75 g) was purified by chromatography on a silica gel column eluted with a mixture of hexane (23 parts by volume) and ethyl acetate (2 parts by volume) to yield (RS)-1,1,1-trifluoro-2-(4-ethoxyphenyl)-3-(3-phenoxybenzyloxy)propane (0.21 g) as a viscous oil.

WORKUP

后处理

  1. customwas partitioned between water and diethyl ether
  2. customThe ethereal phase was separated
  3. washwashed twice with water
  4. dry with materialdried over anhydrous magnesium sulphate
  5. concentrationconcentrated by evaporation of the solvent under reduced pressure
  6. customThe residual oil (0.75 g) was purified by chromatography on a silica gel column
  7. washeluted with a mixture of hexane (23 parts by volume) and ethyl acetate (2 parts by volume)