反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
E-2 1,2-Dihydro-5-methyl-2-oxo-1,6-naphthyridine-3carboxamide--To 200 ml of concentrated sulfuric acid chilled in an ice bath was added with stirring 37 g of 1,2-dihydro-5-methyl-2-oxo-1,6-naphthyridine-3-carbonitrile and the reaction mixture was allowed to stand at room temperature overnight. The reaction mixture was then poured on ice (1 liter beaker, half filled), the resulting mixture cooled in an ice bath and then neutralized by adding aqueous ammonium hydroxide, followed by addition of acetic acid to make the mixture slightly acidic. The separated solid was collected, washed with water, air-dried, then recrystallized from a large volume of dimethylformamide (1.2 1.) and dried at 95° C. to yield 8.4 g of 1,2-dihydro-5-methyl-2-oxo-1,6-naphthyridine-3-carboxamide, m.p.>320° C.
WORKUP
后处理
- additionwas added
- additionThe reaction mixture was then poured on ice (1 liter beaker, half filled)
- temperaturethe resulting mixture cooled in an ice bath
- customThe separated solid was collected
- washwashed with water
- customair-dried
- customrecrystallized from a large volume of dimethylformamide (1.2 1.)
- customdried at 95° C.