HRID1161693

反应详情

EQUATION

反应方程式

HRID 1161693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of compound 4-(2-amino-6-phenyl-pyrimidin-4-ylamino)-2-chloro-phenol (0.5 g, 1.6 mmol) in dry dimethylformamide (10 mL) was added 4-(N,N-dimethylamino)pyridine (0.39 g, 3.2 mmol) at 0° C. with stirring under nitrogen atmosphere. To this was added freshly prepared succinyl chloride (0.62 g, 4 mmol). The mixture was then stirred at 80° C. for 20 hours. After completion of the reaction the mixture was diluted with water (75 mL), the solid separated was filtered off, washed with cold water (200 mL) and dried. The solid was purified further by column chromatography using petroleum ether-ethyl acetate to give the desired product as a light brown solid.

WORKUP

后处理

  1. stirringThe mixture was then stirred at 80° C. for 20 hours
  2. customAfter completion of the reaction the mixture
  3. customthe solid separated
  4. filtrationwas filtered off
  5. washwashed with cold water (200 mL)
  6. customdried
  7. customThe solid was purified further by column chromatography