HRID1032478

反应详情

EQUATION

反应方程式

HRID 1032478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

With stirring, 20 g of methyl α-methylcarbonyl-2,3-dichlorocinnamate are added at 0° C. to a 22 % by weight solution of (p-tolylsulfonyl)methyl isocyanide prepared according to Example P1 (a). Then 26.3 g of a 30% solution of sodium methylate in methanol are added dropwise over 2 hours. The mixture is stirred for 2 hours and then 35 ml of water are added dropwise. The reaction mixture is concentrated at +50° C. under vacuum. After addition of 70 ml of water, the reaction mixture is concentrated once more under vacuum and then filtered. The filter residue is washed with toluene and recrystallised from ethanol, affording 10.8 g (58% of theory) of 4-methoxycarbonyl-3-(2,3-dichlorophenyl)-pyrrole which melts at 200°-201° C.

WORKUP

后处理

  1. customprepared
  2. stirringThe mixture is stirred for 2 hours
  3. concentrationThe reaction mixture is concentrated at +50° C. under vacuum
  4. additionAfter addition of 70 ml of water
  5. concentrationthe reaction mixture is concentrated once more under vacuum
  6. filtrationfiltered
  7. washThe filter residue is washed with toluene
  8. customrecrystallised from ethanol