HRID460032

反应详情

EQUATION

反应方程式

HRID 460032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of bis-(2-methoxyethyl)aminosulfur trifluoride (0.031 g) in anhydrous dichloromethane (0.05 ml) at −78° C. under nitrogen was added a solution of ethyl [4-(1-hydroxy-2-{4-methyl-2-[4-(trifluoromethyl)phenyl]-1,3-thiazol-5-yl}ethyl)-2-methylphenoxy]acetate (intermediate 16, 0.061 g) in anhydrous dichloromethane (1 ml). After two hours at −78° C. the reaction was quenched with saturated sodium bicarbonate solution (2.5 ml) and the product extracted into dichloromethane. The organic extract was separated by hydrophobic frit and evaporated to yield a yellow oil. Purification by flash column chromatography using neat cyclohexane and ethyl acetate:cyclohexane (1:9) as eluents to give the title compound as a yellow solid.

WORKUP

后处理

  1. customAfter two hours at −78° C. the reaction was quenched with saturated sodium bicarbonate solution (2.5 ml)
  2. extractionthe product extracted into dichloromethane
  3. extractionThe organic extract
  4. customwas separated by hydrophobic frit
  5. customevaporated
  6. customto yield a yellow oil
  7. customPurification by flash column chromatography