HRID496747

反应详情

EQUATION

反应方程式

HRID 496747 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of toluene-4-sulfonic acid 7-oxo-7H-5,9-diaza-benzo[c]fluoren-6-yl ester (102 mg) (the compound of Reference Example 6c-2) and N,N′-bis-(2-amino-ethyl)-N,N′-dimethyl-propane-1,3-diamine (0.8 ml) was stirred at 50° C. for 20 minutes. The reaction mixture was diluted with dichloromethane. The solution was washed with saturated NaHCO3 solution and dried over magnesium sulfate. The organic layer was evaporated to dryness. The residue was purified by silica gel column chromatography developed by dichloromethane-methanol-ammonia water (25%)=90:10:1. The desired product (37 mg) was obtained as a reddish oil.

WORKUP

后处理

  1. washThe solution was washed with saturated NaHCO3 solution
  2. dry with materialdried over magnesium sulfate
  3. customThe organic layer was evaporated to dryness
  4. customThe residue was purified by silica gel column chromatography