HRID459119
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was cooled
- concentrationconcentrated to dryness
- washwashed with HCl 1N, and NaHCO3
- customDry over MsSO4
- concentrationconcentrated in vacuo
- customto give a crude that
- customwas purified by silica gel chromatography
- customto give a diastereomeric mixture which
- customwas separated