HRID257787

反应详情

EQUATION

反应方程式

HRID 257787 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1-(3-Nitrophenyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (12.0 g, 42.2 mmoles) was added into 2 liters of acetone and warmed with stirring until a solution was formed. To the solution was added powdered potassium carbonate (23.4 g, 169.3 mmoles) and 4-chloromethylpyridine hydrochloride (10.4 g, 63.4 mmoles). The solution was stirred at reflux temperature for 18 hours. The solution was filtered while hot. Three quarters of the solvent was removed resulting in the formation of a precipitate. The solution was cooled to 0° C. and the precipitate was removed by filtration. The precipitate was washed with ethyl ether and air dried yielding 10.0 g (26.6 mmole, 63% yield) of 1-(3-nitrophenyl)-3-(4-pyridylmethyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (mp 207°-209° C.).

WORKUP

后处理

  1. temperaturewarmed
  2. customwas formed
  3. stirringThe solution was stirred
  4. temperatureat reflux temperature for 18 hours
  5. filtrationThe solution was filtered while hot
  6. customThree quarters of the solvent was removed
  7. customresulting in the formation of a precipitate
  8. customthe precipitate was removed by filtration
  9. washThe precipitate was washed with ethyl ether and air
  10. customdried