HRID478691

反应详情

EQUATION

反应方程式

HRID 478691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture is refluxed, under argon, for 3 days
  2. additionslowly hydrolysed by the addition of ice
  3. customThe precipitate formed
  4. filtrationis filtered off
  5. customdried
  6. customis chromatographed over silica gel (dichloromethane/methanol: gradient from 0.1 to 0.5%)
  7. customto be isolated