HRID1740645
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A suspension of 1-(2-chloro-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene (3.90 g) in hydrazine hydrate (17.8 ml) is refluxed for 9 hours. The mixture is stirred at room temperature for 10 minutes, and further stirred under ice-cooling for 10 minutes. To the mixture are added methylene chloride and water, and the methylene chloride layer is separated, washed, dried, and concentrated under reduced pressure to remove the solvent. The residue is dissolved in hot ethanol (20 ml), and allowed to cool overnight to give 1-(2-hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene (3.19 g).
WORKUP
后处理
- temperatureis refluxed for 9 hours
- stirringfurther stirred under ice-
- temperaturecooling for 10 minutes
- customthe methylene chloride layer is separated
- washwashed
- customdried
- concentrationconcentrated under reduced pressure
- customto remove the solvent
- dissolutionThe residue is dissolved in hot ethanol (20 ml)
- temperatureto cool overnight