HRID1898792
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringAfter stirring
- temperatureunder reflux for 12 hours
- concentrationthe reaction mixture was concentrated
- extractionthe solution was extracted with water
- customThe organic phase was dried
- filtrationfiltered off with suction through neutral alumina
- concentrationconcentrated under reduced pressure
- stirringThe residue was stirred in ether/pentane
- filtrationfiltered off with suction
- customdried