HRID2070240
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
A solution of 0.49 g (1.5 mmol) of 4-(4-cyclohexylphenoxy)-2,5-dimethylnitrobenzene in 7 ml of dioxane and 7 ml of hydrochloric acid is admixed with 1.01 g (4.5 mmol) of tin(II) chloride dihydrate at room temperature and the mixture is then refluxed for 2 h. It is cooled to room temperature, neutralized with aqueous NaHCO3 and extracted repeatedly with dichloromethane, and the extracts are dried over Na2SO4 and filtered, and the solvent is removed under reduced pressure. This is followed by purification by column chromatography (0.29 g, purity 95.2%, yield 61.5%, log P (pH 2.3)=4.25).
WORKUP
后处理
- temperaturethe mixture is then refluxed for 2 h
- extractionextracted repeatedly with dichloromethane
- dry with materialthe extracts are dried over Na2SO4
- filtrationfiltered
- customthe solvent is removed under reduced pressure
- customThis is followed by purification by column chromatography (0.29 g, purity 95.2%, yield 61.5%, log P (pH 2.3)=4.25)