HRID330397

反应详情

EQUATION

反应方程式

HRID 330397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperaturewas refluxed for 16 hr
  2. filtrationThe reaction mixture solution was filtered
  3. customthe solvent was removed in vacuo
  4. customThe residue was partitioned between methylene chloride and dilute sodium hydroxide
  5. dry with materialThe methylene chloride solution was dried over sodium sulfate
  6. customthe solvent was removed in vacuo
  7. customto give an oil
  8. customa whie solid precipitated