HRID1995

反应详情

EQUATION

反应方程式

HRID 1995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

16.8 g (0.7 mol) of sodium hydride were introduced in portions with stirring into a suspension of 99.6 g (0.6 mol) of 3-methylxanthine in 1.5 l of dimethylformamide. After evolution of hydrogen had ended, the mixture was heated to 100° C., treated dropwise with 76 g (0.6 mol) of benzyl chloride and heated at 120° C. for a further 6 hours. The reaction mixture was cooled and cautiously poured into 3 l of water. The solid was filtered off with suction and washed with water, the filter residue was taken up in ethanol and the solution was stirred at room temperature for one hour. The crystallizate was filtered, washed with ethanol and dried under reduced pressure.

WORKUP

后处理

  1. temperatureheated at 120° C. for a further 6 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationThe solid was filtered off with suction
  4. washwashed with water
  5. filtrationThe crystallizate was filtered
  6. washwashed with ethanol
  7. customdried under reduced pressure