HRID224625

反应详情

EQUATION

反应方程式

HRID 224625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 3.6 g of sodium hydride in 100 ml of dry benzene 15.3 g of 3-(dimethylamino)propanol are added and the mixture is refluxed for 6 hours. After this time, 28.6 g of 5-chloro-8-ethyl-2-methyl-8H-pyrazolo[1,5-a]-pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidine are added in small portions with stirring. The solution is refluxed for 10 hours, and then the solvent is distilled off. The residue is treated with water, filtered off and recrystallized from ethyl acetate, yield 25 g (71%); m.p. 62°-64°.

WORKUP

后处理

  1. additionare added
  2. temperaturethe mixture is refluxed for 6 hours
  3. temperatureThe solution is refluxed for 10 hours
  4. distillationthe solvent is distilled off
  5. additionThe residue is treated with water
  6. filtrationfiltered off
  7. customrecrystallized from ethyl acetate, yield 25 g (71%)