HRID2202588

反应详情

EQUATION

反应方程式

HRID 2202588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, 4-(tert-butyldimethylsilyloxymethyl)pyridine (1.1 g, 5 mmol) synthesized in Production Example 84 was dissolved in dichloromethane, and m-chloroperbenzoic acid (1.9 g, 14.5 mmol) was added slowly thereto under an ice cooling. The mixture was heated slowly to a room temperature and then stirred overnight. After the completion of the reaction was confirmed by HPLC, an excess of m-chloroperbenzoic acid was removed by a sodium thiosulfate solution. The remaining mixture was washed with 2-N sodium hydroxide 3 times. The organic layer was dried over magnesium sulfate, and the solvent was distilled off. Thus the title compound (1.2 g, 100%) was obtained as an oily substance.

WORKUP

后处理

  1. customan excess of m-chloroperbenzoic acid was removed by a sodium thiosulfate solution
  2. washThe remaining mixture was washed with 2-N sodium hydroxide 3 times
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. distillationthe solvent was distilled off