HRID579936

反应详情

EQUATION

反应方程式

HRID 579936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

After adding 100 ml of benzene to a diethyl ether solution of methylmagnesium iodide prepared from 1.7 g of magnesium, 9.9 g of methyl iodide, and 100 ml of diethyl ether, 16.6 of 4,4'-bis-dimethylaminobenzophenone was gradually added thereto. After stirring at room temperature for 10 hours, the reaction mixture was decomposed by a saturated aqueous ammonium chloride solution, followed by stirring as it was for 2 hours. After separating and water-washing an organic layer, the solvent was distilled off, and the residue was recrystallized from ethanol to obtain 10.7 g of 1,1-bis(4'-dimethylaminophenyl)ethylene. The melting point was 121° to 122° C., and the theoretical yield was 65%.

WORKUP

后处理

  1. additionwas gradually added
  2. stirringby stirring as it
  3. waitwas for 2 hours
  4. customAfter separating
  5. washwater-washing an organic layer
  6. distillationthe solvent was distilled off
  7. customthe residue was recrystallized from ethanol