HRID462712

反应详情

EQUATION

反应方程式

HRID 462712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added
  2. additionThe reaction mixture was then poured on ice (1 liter beaker, half filled)
  3. temperaturethe resulting mixture cooled in an ice bath
  4. customThe separated solid was collected
  5. washwashed with water
  6. customair-dried
  7. customrecrystallized from a large volume of dimethylformamide (1.2 1.)
  8. customdried at 95° C.