HRID2052

反应详情

EQUATION

反应方程式

HRID 2052 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

3.2 g (0.1315 mol) of sodium hydride were added in portions to a suspension of 30 g (0.1315 mol) of 3-phenylxanthine in 600 ml of DMF, the mixture was stirred at 25° C. for 30 minutes and then heated to 80° C. 27 g (0.1578 mol) of benzyl bromide were then added and the solution was left at 80° C. for 6 hours. After cooling to 50° C., the reaction mixture was poured into 2000 ml of ice-water, and the precipitate obtained was filtered off with suction, washed well with water and dried under reduced pressure. The dry residue was crystallized from dioxane/methanol.

WORKUP

后处理

  1. temperatureheated to 80° C
  2. waitthe solution was left at 80° C. for 6 hours
  3. temperatureAfter cooling to 50° C.
  4. customthe precipitate obtained
  5. filtrationwas filtered off with suction
  6. washwashed well with water
  7. customdried under reduced pressure
  8. customThe dry residue was crystallized from dioxane/methanol