HRID1028436
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 mixture of 1.00 g 5-tert-butyl-2-methoxy-1-methylsulphanylmethyl-3-nitro-benzene, 4.20 g tin dichloride dihydrate and 15 ml of ethanol is refluxed for 2 h. Then the solvent is removed, and water and dichloromethane are added to the residue. The mixture is filtered through Celite, and the aqueous part of the filtrate is separated off and extracted twice with dichloromethane. The combined organic phases are dried (Na2SO4), and the solvent is removed. The residue is chromatographed on aluminium oxide with cyclohexane/ethyl acetate (4:1→1:4) as eluant.
WORKUP
后处理
- temperatureis refluxed for 2 h
- customThen the solvent is removed
- additionwater and dichloromethane are added to the residue
- filtrationThe mixture is filtered through Celite
- customthe aqueous part of the filtrate is separated off
- extractionextracted twice with dichloromethane
- dry with materialThe combined organic phases are dried (Na2SO4)
- customthe solvent is removed
- customThe residue is chromatographed on aluminium oxide with cyclohexane/ethyl acetate (4:1→1:4) as eluant