HRID1898792

反应详情

EQUATION

反应方程式

HRID 1898792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.7 g (0.1 mol) of benzylamine and 10.1 g (0.1 mol) of triethylamine were added to a mixture of 25.8 g (0.1 mol) of diethyl 6-chloropyridine-2,3-dicarboxylate in 250 ml of propanol at 25° C. with stirring in the course of 10 minutes. After stirring under reflux for 12 hours, the reaction mixture was concentrated, the residue was taken up in methylene chloride and the solution was extracted with water. The organic phase was dried, filtered off with suction through neutral alumina and concentrated under reduced pressure. The residue was stirred in ether/pentane, filtered off with suction and dried, 23.3 g (71.1% of theory) of the title compound of m.p. 110°-114° C. being obtained.

WORKUP

后处理

  1. stirringAfter stirring
  2. temperatureunder reflux for 12 hours
  3. concentrationthe reaction mixture was concentrated
  4. extractionthe solution was extracted with water
  5. customThe organic phase was dried
  6. filtrationfiltered off with suction through neutral alumina
  7. concentrationconcentrated under reduced pressure
  8. stirringThe residue was stirred in ether/pentane
  9. filtrationfiltered off with suction
  10. customdried