HRID2196111

反应详情

EQUATION

反应方程式

HRID 2196111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution 2-(3,5-Dichloropyridin-4-yl)-1-{9-methoxy-spiro[2H-1,5-benzodioxepin-3(4H),4′-tetrahydropyran]-6-yl}ethanone [127] (66 mg, 150 μmmol) in CH2Cl2 (2 mL) was added 30% H2O2 (45 μL) and methyltrioxorhenium(VII) (10 mg). The mixture was stirred for 18 h, added MnO2 (10 mg) and was stirred for another hour. CH2Cl2 (10 mL) was added and the organic phase was washed with water. The combined organic phase was dried over MgSO4 and evaporated to dryness under reduced pressure. Standard HPLC purification afforded 5.6 mg of the product.

WORKUP

后处理

  1. stirringwas stirred for another hour
  2. washthe organic phase was washed with water
  3. dry with materialThe combined organic phase was dried over MgSO4
  4. customevaporated to dryness under reduced pressure
  5. customStandard HPLC purification