HRID1585700

反应详情

EQUATION

反应方程式

HRID 1585700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

0.27 g (0.0009 mol) of 4-amino-N-(2-amino-6-chloro-pyrimidin-4-yl)-benzenesulfonamide was dissolved in a solution of 0.23 g of sodium in 20 ml of methanol and stirred in an autoclave at 150° C. for 9 hours. The solvent was distilled off, the residue was added to water and the pH value was adjusted to 4-5 with 1N HCl. The precipitate which thereby separated was filtered off under suction, washed with water and dried. The crystals obtained were triturated in 20 ml of methanol, again filtered off and dried in a high vacuum. There was obtained 0.25 g (94%) of 4-amino-N-(2-amino-6-methoxy-pyrimidin-4-yl)-benzenesulfonamide as beige crystals; m.p.: >250° C. (dec.).

WORKUP

后处理

  1. distillationThe solvent was distilled off
  2. additionthe residue was added to water
  3. customThe precipitate which thereby separated
  4. filtrationwas filtered off under suction
  5. washwashed with water
  6. customdried
  7. customThe crystals obtained
  8. customwere triturated in 20 ml of methanol
  9. filtrationagain filtered off
  10. customdried in a high vacuum