HRID386023
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
6-Chloro-2-methylnicotinaldehyde (1 g, 6.43 mmol), hydroxylamine hydrochloride (0.45 g, 6.43 mmol), and sodium acetate (0.53 g, 6.43 mmol) were dissolved in dry ethanol (32 ml) and transferred to a flame-dried round bottom flask. The reaction was allowed to stir at room temperature for 20 minutes. It was then concentrated under reduced pressure, re-dissolved in ethyl acetate, and washed with water. The aqueous layer was extracted with ethyl acetate two times. The organic layers were combined, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Purification was performed via silica gel chromatography (0-100% ethyl acetate in hexane) to afford the title compound.
WORKUP
后处理
- customtransferred to a flame-dried round bottom flask
- concentrationIt was then concentrated under reduced pressure
- dissolutionre-dissolved in ethyl acetate
- washwashed with water
- extractionThe aqueous layer was extracted with ethyl acetate two times
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customPurification