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 20.0 g (0.106 mole) of [(2-chloroethyl)sulfinyl]benzene, 30.0 g (0.259 mole) of N,N-diethylethylenediamine and excess sodium carbonate in 600 ml of acetonitrile was refluxed for 16 hr. The reaction mixture solution was filtered, and the solvent was removed in vacuo. The residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over sodium sulfate and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and a solution of 2 equivalents of maleic acid in methanol was added. Diethyl ether was added and a whie solid precipitated to give 26.7 g (50.3%) of title compound, a white crystalline solid, mp 111°-112.5° C.
WORKUP
后处理
- temperaturewas refluxed for 16 hr
- filtrationThe reaction mixture solution was filtered
- customthe solvent was removed in vacuo
- customThe residue was partitioned between methylene chloride and dilute sodium hydroxide
- dry with materialThe methylene chloride solution was dried over sodium sulfate
- customthe solvent was removed in vacuo
- customto give an oil
- customa whie solid precipitated