HRID1987

反应详情

EQUATION

反应方程式

HRID 1987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

52.5 g (0.28 mol) of p-toluenesulfonyl chloride were initially introduced into 50 ml of dimethylformamide and 22.6 g (0.29 mol) of sodium acetate were introduced with stirring and ice-cooling. The mixture was subsequently stirred for one hour, treated with 39.1 g of formaldehyde diethyl acetal and again subsequently stirred for one hour. 41.5 g of 3-methylxanthine were then introduced and the reaction mixture was heated at 90° C. for 2 hours. After cooling to 10° C., the precipitated product was filtered off with suction, washed with a little dimethylformamide and washed with demineralized water until chloride-free. The crude product obtained was recrystallized from dimethylformamide.

WORKUP

后处理

  1. additionwere introduced
  2. temperatureice-cooling
  3. stirringThe mixture was subsequently stirred for one hour
  4. stirringagain subsequently stirred for one hour
  5. temperatureAfter cooling to 10° C.
  6. filtrationthe precipitated product was filtered off with suction
  7. washwashed with a little dimethylformamide
  8. washwashed with demineralized water until chloride-free