HRID4193

反应详情

EQUATION

反应方程式

HRID 4193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 32.86 g (0.177 mole) of 1-chloro-3-(phenylthio)propane and 33.7 g (0.182 mole) of potassium phthalimide in 500 ml of dimethylformamide was stirred at 80° C. for 19 hr. The dimethylformamide was removed in vacuo. The residue was dissolved in methylene chloride and the resulting solution extracted with several portions of dilute sodium hydroxide solution. The methylene chloride layer was dried over magnesium sulfate, filtered, and the filtrate evaporated in vacuo. The resulting solid residue was recrystallized from methylene chloride-hexane to give 33.56 g (63.8%) of white crystalline product, m.p. 83°-85° C.

WORKUP

后处理

  1. customThe dimethylformamide was removed in vacuo
  2. dissolutionThe residue was dissolved in methylene chloride
  3. extractionthe resulting solution extracted with several portions of dilute sodium hydroxide solution
  4. dry with materialThe methylene chloride layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate evaporated in vacuo
  7. customThe resulting solid residue was recrystallized from methylene chloride-hexane