HRID1656806

反应详情

EQUATION

反应方程式

HRID 1656806 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.8 milliliters KN(SiCH3)2 were dropped into 5 milliliters (C6H5)2CHCOOCH3 in tetrahydrofuran at -78° C. and the resulting yellow suspension was stirred for 45 minutes. 1.2 molar equivalents N-fluorobenzenesulfonimide prepared according to Example 1 above in 4 milliliters tetrahydrofuran were dropped into the mixture and stirring continued at -78° C. for 1 hour. The mixture was allowed to warm up to room temperature, quenched with ammonium chloride, and acidified with 0.1N hydrogen chloride. Extraction with dichloromethane, drying, and evaporation were followed by purification on a silica gel column. White crystalline (C6H5)2CFCOOCH3 was obtained in 82% yield.

WORKUP

后处理

  1. additionwere dropped into the mixture
  2. stirringstirring
  3. waitcontinued at -78° C. for 1 hour
  4. customquenched with ammonium chloride
  5. extractionExtraction with dichloromethane
  6. customdrying
  7. customevaporation
  8. customwere followed by purification on a silica gel column