HRID636540

反应详情

EQUATION

反应方程式

HRID 636540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.5 g (3.8 mmol) of the compound from Example IV are dissolved in 350 ml of CH2Cl2 and treated with 7.5 g of MnO2. The mixture is kept under reflux for 2 h, solid is filtered off with suction through Celite and the filtrate is concentrated. The residue is purified by MPLC (methylene chloride/ethyl acetate 10+1). After recrystallization, first from ether/petroleum ether and then from isopropanol/petroleum ether, 0.72 g (48% of theory) of the title compound is obtained.

WORKUP

后处理

  1. temperatureunder reflux for 2 h
  2. filtrationsolid is filtered off with suction through Celite
  3. concentrationthe filtrate is concentrated
  4. customThe residue is purified by MPLC (methylene chloride/ethyl acetate 10+1)
  5. customAfter recrystallization