HRID1931561

反应详情

EQUATION

反应方程式

HRID 1931561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,4-difluoro-nitrobenzene (25 g, 0.157 mol) and sodium methanethiolate (10.5 g, 0.15 mol) was stirred at room temperature overnight. The reaction mixture was poured into water and extracted twice with ether. The extracts were combined, washed with water (twice) and brine, dried (sodium sulfate), filtered, evaporated, and purified by column chromatography, eluting with 17% dichloromethane/hexanes to give 2-fluoro-1-methylsulfanyl-4-nitro-benzene (18.6 g, 63%).

WORKUP

后处理

  1. extractionextracted twice with ether
  2. washwashed with water (twice) and brine
  3. dry with materialdried (sodium sulfate)
  4. filtrationfiltered
  5. customevaporated
  6. custompurified by column chromatography
  7. washeluting with 17% dichloromethane/hexanes