HRID992447

反应详情

EQUATION

反应方程式

HRID 992447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

41 ml of a 30% solution of sodium methylate in methanol are added to a solution of 31.5 g (180 mmol) N-[2-(4-hydroxy-3-methoxy-phenyl)-ethyl]-formamide in 880 ml methanol. 48.1 g (184 mmol) toluene-4-sulfonic acid pent-2-ynyl ester are added and the mixture is refluxed for 4 hours. After evaporation the residue is taken up in ethyl acetate and washed with water. After evaporation the residue is submitted to flash-chromatography and crystallisation in ether to give the N-[2-(3-methoxy-4-pent-2-ynyloxy-phenyl)-ethyl]-formamide.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 4 hours
  2. customAfter evaporation the residue
  3. washwashed with water
  4. customAfter evaporation the residue
  5. customis submitted to flash-chromatography and crystallisation in ether