HRID1993719
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
1.98 g of 1-(2,4-dihydroxyphenyl)ethanone oxime (12 mM) and 1 g of potassium hydroxide (18 mM) are refluxed for 4 days in a methanol/water mixture (100 ml/100 ml). The reaction medium is subsequently concentrated under reduced pressure, acidified to pH=1 with 1N HCl, and then extracted with ethyl acetate. The organic phase obtained is dried over magnesium sulfate and concentrated under reduced pressure. The evaporation residue is purified by silica gel chromatography (methylcyclohexane/ethyl acetate gradient of 70/30 to 30/70; v/v). The expected product is obtained in the form of a white solid (0.39 g) with a yield of 22%.
WORKUP
后处理
- concentrationThe reaction medium is subsequently concentrated under reduced pressure
- extractionextracted with ethyl acetate
- customThe organic phase obtained
- dry with materialis dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe evaporation residue is purified by silica gel chromatography (methylcyclohexane/ethyl acetate gradient of 70/30 to 30/70; v/v)