HRID1719651

反应详情

EQUATION

反应方程式

HRID 1719651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

270 g of 5-(2,6-dichloro-4-trifluoromethylphenoxy)-2-nitro-benzaldehyde and 6 g of piperidine were added, at 25° C., to 89.5 g of malonic acid in 570 ml of pyridine. The reaction mixture was stirred for 5 hours at 85° to 90° C. and was then heated for 90 minutes under reflux, after which it was poured onto water, the mixture was acidified with hydrochloric acid and the product was filtered off. The crystalline product was recrystallized from n-butanol. 200 g (66% of theory) of 3-(5-(2,6-dichloro-4-trifluoromethyl-phenoxy)-2-nitrophenyl)propenoic acid, of melting point 192° C., were obtained in the form of yellow crystals.

WORKUP

后处理

  1. temperaturewas then heated for 90 minutes
  2. temperatureunder reflux
  3. additionafter which it was poured onto water
  4. filtrationthe product was filtered off
  5. customThe crystalline product was recrystallized from n-butanol