HRID1750228

反应详情

EQUATION

反应方程式

HRID 1750228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the solution of 180 g of) 7-(Toluene-4-sulfonyl)-7-aza-bicyclo[4.1.0]heptane and 18 g of Copper(II)acetyl acetonate in 1500 ml of dry THF was added 86 ml of a 10 M solution of methyllithium dropwise over 30 min. The mixture was stirred under nitrogen atmosphere for 8 h. It was then washed with water and extracted with ethyl acetate twice. The combined organic layers were concentrated. The resulting residue was purified by chromatography (silica, hexan/ethyl acetate) to afford 120 g (62%) of 4-Methyl-N-(trans-2-methyl-cyclohexyl)-benzenesulfonamide

WORKUP

后处理

  1. washIt was then washed with water
  2. extractionextracted with ethyl acetate twice
  3. concentrationThe combined organic layers were concentrated
  4. customThe resulting residue was purified by chromatography (silica, hexan/ethyl acetate)