HRID1680548

反应详情

EQUATION

反应方程式

HRID 1680548 的结构方程式

PROCEDURE

实验过程

Into a 200 ml, one-neck flask is placed 35 grams of sodium methyl maleate (0.23 moles), 85 grams (0.73 moles) of phenyl acetonitrile and 80 g (1.1 moles) dimethyl formamide. The reaction mixture is heated to 135°-140° C. for five hours and then distilled in vacuo. The residue is extracted three time with 300 ml ether. The solid (56 grams) is then dissolved in water and acidified with 23 grams conc. HCl in 50 mls water. The liquid that separates out is dissolved in ether and washed with water to remove unreacted starting materials. The ether is distilled off to give a residue of 50 grams of product (yield: 88%). The structure is verified by NMR (in CDCl3): ##STR37##

WORKUP

后处理

  1. temperatureThe reaction mixture is heated to 135°-140° C. for five hours
  2. distillationdistilled in vacuo
  3. extractionThe residue is extracted three time with 300 ml ether
  4. dissolutionThe solid (56 grams) is then dissolved in water
  5. dissolutionThe liquid that separates out is dissolved in ether
  6. washwashed with water
  7. customto remove unreacted
  8. distillationThe ether is distilled off