HRID978959

反应详情

EQUATION

反应方程式

HRID 978959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 16 parts of ethyl toluene-4-sulfonate in 15 parts of dimethylformamide is added to a mixture, warmed to 140°-142° C., of 5.8 parts of 1,4-diketo-3,6-diphenylpyrrolo-[3,4-c]-pyrrole, 12.2 parts of potassium carbonate and 60 parts of dimethylformamide in the course of 30 minutes, with stirring. The brown-yellow solution formed is subsequently stirred at 142° C. for 5 minutes, and 100 parts of methanol are added at 70° C. The yellow precipitate which has separated out is filtered off at 15° C., washed with methanol and with hot water at 90° C. and dried. The crude product (3.6 parts) is recrystallised first from 40 part of dimethylformamide and then from 100 parts of n-butanol. 2.8 parts of 1,4-diketo-2,5-diethyl-3,6-diphenylpyrrolo-[3,4-c]-pyrrole of the following formula are obtained in the form of orange-yellow needles of melting point 229°-230° C.: ##STR32##

WORKUP

后处理

  1. customThe brown-yellow solution formed
  2. stirringis subsequently stirred at 142° C. for 5 minutes
  3. customThe yellow precipitate which has separated out
  4. filtrationis filtered off at 15° C.
  5. washwashed with methanol and with hot water at 90° C.
  6. customdried
  7. customThe crude product (3.6 parts) is recrystallised first from 40 part of dimethylformamide