HRID636540
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 2 h
- filtrationsolid is filtered off with suction through Celite
- concentrationthe filtrate is concentrated
- customThe residue is purified by MPLC (methylene chloride/ethyl acetate 10+1)
- customAfter recrystallization