HRID2233577

反应详情

EQUATION

反应方程式

HRID 2233577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.1 g crude 4-Butyl-5-(3-chloro-4-chloromethyl-phenoxymethyl)-2-(4-trifluoromethyl-phenyl)-thiazole was dissolved in 50 ml acetonitrile. 2.0 g tetrabutylammonium cyanide were added and the reaction mixture stirred at room temperature for one hour. Then a mixture of saturated NaHCO3 solution, ice and ethyl acetate was added. The aqueous phase was separated and extracted three times with portions of 30 ml ethylacetate. The combined organic layers were washed with ice cold water and brine and dried over MgSO4. The solvent was removed in vacuo. The residue was purified by flash chromatography with the eluent n-heptane:ethyl acetate=4:1 to provide 2.2 g {4-[4-Butyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-2-chloro-phenyl}-acetonitrile as oil.

WORKUP

后处理

  1. additionwas added
  2. customThe aqueous phase was separated
  3. extractionextracted three times with portions of 30 ml ethylacetate
  4. washThe combined organic layers were washed with ice cold water and brine
  5. dry with materialdried over MgSO4
  6. customThe solvent was removed in vacuo
  7. customThe residue was purified by flash chromatography with the eluent n-heptane