HRID1836841

反应详情

EQUATION

反应方程式

HRID 1836841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

The compound (46 mg) prepared in step (d) of Example 133 was dissolved in dichloromethane (1 ml). m-Chloroperbenzoic acid (19 mg) was added to the solution at 0° C., and the mixture was stirred at 0° C. for one hr. Water was added to the reaction solution, and the mixture was extracted with chloroform. The extract was dried over anhydrous MgSO4, and the solvent was then removed by distillation under the reduced pressure. The residue was purified by preparative TLC (n-hexane:ethyl acetate=1:4) to give 4-[10-oxo-9-(2,2,2-trifluoroethylcarbamoyl)-9,10-dihydro-10λ4-thioxanthen-9-yl]butyl bromide (38 mg).

WORKUP

后处理

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe extract was dried over anhydrous MgSO4
  3. customthe solvent was then removed by distillation under the reduced pressure
  4. customThe residue was purified by preparative TLC (n-hexane:ethyl acetate=1:4)