HRID459119

反应详情

EQUATION

反应方程式

HRID 459119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
36 °C

PROCEDURE

实验过程

A mixture of (1R*,3S*)-3-(Biphenyl-4-yloxy)-cyclohexanol from Step C (1 eq) with (S)-(−)-α-methoxy-α-(trifluoromethyl)-phenylacetic acid (1 eq), DMAP (0.1 eq) and EDCI (1.2 eq) in dichloromethane was stirred at 36° C. over night. The reaction mixture was cooled and concentrated to dryness. Reconstituted in: ether and washed with HCl 1N, and NaHCO3. Dry over MsSO4 and concentrated in vacuo to give a crude that was purified by silica gel chromatography to give a diastereomeric mixture which was separated using chiral HPLC

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. concentrationconcentrated to dryness
  3. washwashed with HCl 1N, and NaHCO3
  4. customDry over MsSO4
  5. concentrationconcentrated in vacuo
  6. customto give a crude that
  7. customwas purified by silica gel chromatography
  8. customto give a diastereomeric mixture which
  9. customwas separated