HRID1906721

反应详情

EQUATION

反应方程式

HRID 1906721 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 8.3 g (0.053 mole) of methyl phenyl sulfoximine in 400 ml of dry tetrahydrofuran at 0° C. was added 1.4M (0.13 mol) butyl lithium in hexane to obtain a clear yellow solution. 15 ml (0.172 mole) of benzonitrile were added and the mixture was stirred for 30 minutes. 100 ml of saturated sodium chloride solution were added and the organic layer was separated, dried over magnesium sulfate and evaporated to an oil. The crude oil was triturated with petrol-ether (40° C.-60° C.) and then was chromatographed over silica. Elution with CH2Cl2, then a 1--1 CH2Cl2 : EtOAc mixture yielded 8.8 g (64% yield) of pure S-(2-aminostyryl)-S-phenyl sulfoximine melting at 95°-96° C. after crystallization from ether.

WORKUP

后处理

  1. customto obtain a clear yellow solution
  2. customthe organic layer was separated
  3. dry with materialdried over magnesium sulfate
  4. customevaporated to an oil
  5. customThe crude oil was triturated with petrol-ether (40° C.-60° C.)
  6. customwas chromatographed over silica
  7. washElution with CH2Cl2