HRID2166753

反应详情

EQUATION

反应方程式

HRID 2166753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

The product from Step B, 2.II, 207 mg, in 9 ml of CH2Cl2 is treated dropwise at 0° C. over 70 minutes with 121 mg of m-chloroperbenzoic acid (MCPBA) (85%) in 9 ml of CH2Cl2 under N2. The solution is stirred 1 hour at 25° C., washed with aqueous NaHCO3, dried with MgSO4, filtered, evaporated (209 mg) and purified by preparative thin layer chromatography on silica gel with 4:1 (v/v) CHCl3 -ethylacetate, affording 97 mg of pure product, Rf 0.25.

WORKUP

后处理

  1. washwashed with aqueous NaHCO3
  2. dry with materialdried with MgSO4
  3. filtrationfiltered
  4. customevaporated (209 mg)
  5. custompurified by preparative thin layer chromatography on silica gel with 4:1 (v/v) CHCl3 -ethylacetate