HRID324485

反应详情

EQUATION

反应方程式

HRID 324485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of the product from step (iv) (0.535 g), and phosphorus pentasulphide (0.967 g) in 1,4-dioxane (10 ml) was heated at 100° C. for 3 h. The solvent evaporated and the residue dissolved in dichloromethane, washed with saturated aqueous sodium bicarbonate solution then with water, dried (MgSO4) and evaporated. Purification was by chromatography on a biotage silica column, using 3% methanol/0.1% 0.880 ammonia in dichloromethane as eluant.

WORKUP

后处理

  1. customThe solvent evaporated
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with saturated aqueous sodium bicarbonate solution
  4. dry with materialwith water, dried (MgSO4)
  5. customevaporated
  6. customPurification