HRID565381

反应详情

EQUATION

反应方程式

HRID 565381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of hydroxylamine hydrochloride (4.17 g) in water (50 ml) was added sodium carbonate (3.18 g) with stirring under ice cooling. To the solution were subsequently added ethanol (200 ml) and 1,2-dihydro-5-methyl-2-oxo-1,6-naphthyridine-3-carbonitrile (3.70 g), and the mixture was refluxed for 2 hours. After distilling off the solvent under reduced pressure, water was added to the residue, and the precipitated crystals were separated by filtration. The product was washed with water, isopropanol, diisopropyl ether in this order, and dried to give 1,2-dihydro-5-methyl-2-oxo-1,6-naphthyridin-3-amidoxime (4.2 g). This compound was used in the next reaction without being purified.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. distillationAfter distilling off the solvent under reduced pressure, water
  3. additionwas added to the residue
  4. customthe precipitated crystals were separated by filtration
  5. washThe product was washed with water, isopropanol, diisopropyl ether in this order
  6. customdried