HRID1285303

反应详情

EQUATION

反应方程式

HRID 1285303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.5 g of 3-cyano-4-(2,3-dichlorophenyl)pyrrole are dissolved in 50 ml of tetrahydrofuran and to the solution are added 0.65 g of paraformaldehyde, 3.0 ml of triethylamine and 0.5 ml of diazobicyclo[5.4.0]undec-7-ene. The mixture is stirred for 2 hours at room temperature to form a clear solution. With stirring, 2.0 ml of ethoxyacetyl chloride are slowly added dropwise at 5° C. The reaction mixture is kept for 21/2 hours at 0°-5° C. and then filtered. The filtrate is concentrated and the residue is crystallised from ether/petroleum ether to give colourless crystals of the title compound with a melting point of 72°-75° C.

WORKUP

后处理

  1. customto form a clear solution
  2. stirringWith stirring
  3. custom2 hours
  4. customat 0°-5° C.
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated
  7. customthe residue is crystallised from ether/petroleum ether