HRID463287

反应详情

EQUATION

反应方程式

HRID 463287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.35 g of 1-[2-chloro-4-(4-chlorophenyl)butyl]imidazole and 1.60 g of 4-nitrobenzyl mercaptan in 40 ml tetrahydrofuran was treated with 380 mg of 50% sodium hydride dispersion in mineral oil. After stirring at room temperature for 1 hour and under reflux for 12 hours the solvent was evaporated under vacuum and 50 ml of ether added. The resulting mixture was washed twice with water and the ethereal solution dried (MgSO4) and evaporated. The residue was chromatographed on silica gel eluting with 5% methanol in methylene chloride to give 1-[4-(4-chlorophenyl)-2-(4-nitrobenzylthio)-n-butyl]imidazole.

WORKUP

后处理

  1. temperatureunder reflux for 12 hours the solvent
  2. customwas evaporated under vacuum and 50 ml of ether
  3. additionadded
  4. washThe resulting mixture was washed twice with water
  5. dry with materialthe ethereal solution dried (MgSO4)
  6. customevaporated
  7. customThe residue was chromatographed on silica gel eluting with 5% methanol in methylene chloride