HRID2263378

反应详情

EQUATION

反应方程式

HRID 2263378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

9.70 g 4-Methyl-2-[2-(4-trifluoromethyl-phenyl)-ethyl]-oxazole-5-carboxylic acid ethyl ester were dissolved in 20 ml tetrahydrofuran and added to a ice cooled solution of 1.13 g lithium aluminium hydride in 10 ml tetrahydrofuran. The reaction mixture was stirred at 0° C. for one hour. Then 100 ml ethyl acetate and 50 ml saturated NH4Cl solution were added. The precipitate was filtered off through a celite pad and washed with ethyl acetate. The organic layer of the filtrate was separated. The aqueous layer of the filtrate was extracted two times with portions of 100 ml ethyl acetate. The combined organic layers were dried over MgSO4. The solvent was removed in vacuo and the residue purified by chromatography on silica gel with the eluent petroleum benzene:ethyl acetate=1:1 to obtain to 4.20 g {4-methyl-2-[2-(4-trifluoromethyl-phenyl)-ethyl]-oxazol-5-yl}-methanol a yellow solid.

WORKUP

后处理

  1. filtrationThe precipitate was filtered off through a celite pad
  2. washwashed with ethyl acetate
  3. customThe organic layer of the filtrate was separated
  4. extractionThe aqueous layer of the filtrate was extracted two times with portions of 100 ml ethyl acetate
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. customThe solvent was removed in vacuo
  7. customthe residue purified by chromatography on silica gel with the eluent petroleum benzene