HRID1081594

反应详情

EQUATION

反应方程式

HRID 1081594 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

2,4-Diamino-6-benzyloxymethyl-5-(2,4-dichlorophenyl)pyrimidine (Example 26) (6.5 g) was dissolved in a 47% solution of hydrobromic acid in acetic acid (75 ml) and the mixture stirred and heated at 100° C. for 6 hours. After standing at room temperature overnight the dihydrobromide salt was filtered off, washed with ether and dried in vacuo, 6 g. To a stirred solution of the dihydrobromide salt (0.43 g) in dimethylsulphoxide (4 ml) was added dropwise a solution of sodium bicarbonate (0.84 g) in water (10 ml). After 30 minutes the precipitate was filtered off washed with water then ether and dried in vacuo, 0.26 g, mp.>270° C. (decomposes).

WORKUP

后处理

  1. filtrationthe dihydrobromide salt was filtered off
  2. washwashed with ether
  3. customdried in vacuo, 6 g
  4. additionTo a stirred solution of the dihydrobromide salt (0.43 g) in dimethylsulphoxide (4 ml) was added dropwise a solution of sodium bicarbonate (0.84 g) in water (10 ml)
  5. filtrationAfter 30 minutes the precipitate was filtered off
  6. washwashed with water
  7. dry with materialether and dried in vacuo, 0.26 g, mp.>270° C. (decomposes)