HRID253171

反应详情

EQUATION

反应方程式

HRID 253171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the minor isomer product of Example 3E (9.3 g, 29.4 mmol) in 40 mL CH2Cl2 at 0° C. was added 20 mL trifluoroacetic acid. The ice bath was removed after the addition and the mixture stirred at ambient temperature for 3 h then was concentrated under reduced pressure and the residue was purified via column chromatography (SiO2, 1% NH4OH:9% CH3OH:90% CH2Cl2) to give the title compound. MS (DCl/NH3) m/z 217 (M+H)+.

WORKUP

后处理

  1. customThe ice bath was removed
  2. additionafter the addition
  3. concentrationthen was concentrated under reduced pressure
  4. customthe residue was purified via column chromatography (SiO2, 1% NH4OH:9% CH3OH:90% CH2Cl2)