HRID750968

反应详情

EQUATION

反应方程式

HRID 750968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14 mg (0.55 mmol) 95% sodium hydride were given to a solution of 126 mg (0.50 mmol) 4-(2-[1,2,3]triazol-1-yl-ethanesulfinylmethyl)-phenol in 4.0 ml DMF and stirred for 15 min. 168 mg (0.50 mmol) 4-Chloromethyl-2-[2-(4-trifluoromethanesulfinyl-phenyl)-vinyl]-oxazole were added and stirring continued at r.t. overnight. After addition of 6 ml water the resulting precipitate was collected and combined with additional material obtained by extraction of the aqueous phase at pH=3 with ethyl acetate, drying (sodium sulfate) and evaporation. Purification by chromatography on silica gel (eluent: ethyl acetate/methanol 9:1) gave 130 mg (77%) powder.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued at r.t. overnight
  3. customwas collected
  4. customobtained by extraction of the aqueous phase at pH=3 with ethyl acetate
  5. customdrying
  6. custom(sodium sulfate) and evaporation
  7. customPurification by chromatography on silica gel (eluent: ethyl acetate/methanol 9:1)