HRID1719228

反应详情

EQUATION

反应方程式

HRID 1719228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-(4-bromo-2-fluorobenzyl)-7-trifluoromethylindoline-2,3-dione (3.35 g.), potassium cyanide (1.06 g.) and ammonium carbonate monohydrate (7.8 g.) in methanol (150 ml.) and water (150 ml.) was heated at 45°-50° C. for 16 hours. The reaction mixture was cooled and a slight precipitate removed by filtration. The filtrate was acidified (2M hydrochloric acid, 80 ml.). The solid which formed was washed with water and recrystallised from tetrahydrofuran (THF)/petrol 60-80 to give 1'-(4-bromo-2-fluorobenzyl)-7'-(trifluoromethyl)-spiro[imidazolidine-4,3'-indoline]-2,2',5-trione (A) (1.98 g.), m.p. 197°-199° C.

WORKUP

后处理

  1. temperaturewas heated at 45°-50° C. for 16 hours
  2. temperatureThe reaction mixture was cooled
  3. customa slight precipitate removed by filtration
  4. customThe solid which formed
  5. washwas washed with water
  6. customrecrystallised from tetrahydrofuran (THF)/petrol 60-80