HRID68627

反应详情

EQUATION

反应方程式

HRID 68627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the compound 6 (225 mg), a solution of 25% trifluoroacetic acid in dichloromethane (6 mL) was added. The reaction mixture was stirred at room temperature for one hour. The reaction mixture was concentrated and the residue was added by 1N sodium hydroxide and then extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and then concentrated. The obtained residue was purified by silica gel column chromatography (dichloromethane:methanol:28% ammonia water=80:10:1) to obtain the title compound (92 mg) having the following physical properties.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionthe residue was added by 1N sodium hydroxide
  3. extractionextracted with dichloromethane
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe obtained residue was purified by silica gel column chromatography (dichloromethane:methanol:28% ammonia water=80:10:1)