HRID1586420

反应详情

EQUATION

反应方程式

HRID 1586420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido-[2,3-d]pyrimidin-7-one, 0.50 g (4.70 mmol) of benzylamine and 0.5 mL of dimethylformamide was heated with stirring in a 120° C. oil bath. After 5 minutes, solution was complete. After 5 hours, the excess amine and dimethylformamide were evaporated at reduced pressure, and the residue was triturated with a solution of 1 mL of acetone and 2 mL of petroleum ether. The tacky solid was filtered and recrystallized from ethyl acetate/petroleum ether to give 0.092 g of pure product; mp 217-219° C.

WORKUP

后处理

  1. temperaturewas heated
  2. waitAfter 5 hours
  3. customthe excess amine and dimethylformamide were evaporated at reduced pressure
  4. customthe residue was triturated with a solution of 1 mL of acetone and 2 mL of petroleum ether
  5. filtrationThe tacky solid was filtered
  6. customrecrystallized from ethyl acetate/petroleum ether