HRID1827907
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
To a solution of 300 mg of the compound obtained in Step 5 in 30 ml of dimethylformamide there are added 1.48 g of sodium hydride and then 1.8 ml of iodomethane. The reaction mixture is refluxed, under argon, for 3 days, and is then slowly hydrolysed by the addition of ice. The precipitate formed is filtered off and then dried and is chromatographed over silica gel (dichloromethane/methanol: gradient from 0.1 to 0.5%), allowing the expected product to be isolated.
WORKUP
后处理
- temperatureThe reaction mixture is refluxed, under argon, for 3 days
- additionslowly hydrolysed by the addition of ice
- customThe precipitate formed
- filtrationis filtered off
- customdried
- customis chromatographed over silica gel (dichloromethane/methanol: gradient from 0.1 to 0.5%)
- customto be isolated