HRID862893

反应详情

EQUATION

反应方程式

HRID 862893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

17.2% by weight of 2,4-dichloronitrobenzene, 15.6% by weight of methyl 5-fluoroanthranilate, 1.5% by weight of Pd--C (5%), 1.0% by weight of 2,4,6-trimethylbenzoic acid and 0.4% by weight of 3,4,7,8-tetramethyl-1,10-phenanthroline are dissolved in 64.3% by weight of toluene and filled into an HC-4 autoclave. A pressure of 100 bar of CO is set and the temperature is increased to 180° C. After 2 hours, the autoclave is allowed to cool, and the product is filtered off together with the active carbon and recrystallized from dichlorobenzene. 51% of 3-(2,4-dichlorophenyl)-6-fluoro-2,4(1H,3H)-quinazolinedione is obtained.

WORKUP

后处理

  1. additionfilled into an HC-4 autoclave
  2. temperatureto cool
  3. filtrationthe product is filtered off together with the active carbon
  4. customrecrystallized from dichlorobenzene