HRID1722252

反应详情

EQUATION

反应方程式

HRID 1722252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 4-hydroxy-7-trifluoromethylquinoline-3-carboxylate (370.5 g), anhydrous potassium carbonate (179.4 g), iodomethane (202.4 g) and anhydrous dimethylformamide (2 liters) was stirred at room temperature overnight. More dimethylformamide (500 ml) was added and stirring was continued for 24 hours. The dimethylformamide was distilled off in vacuo and water (2 litres) was added to the residue. The resulting solid was collected, washed with water, dried and recrystallised from IMS to give the novel compound ethyl 1-methyl-4-oxo-7-trifluoromethyl-1,4-dihydroquinoline-3-carboxylate, m.p. 222°-224°.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 24 hours
  3. distillationThe dimethylformamide was distilled off in vacuo and water (2 litres)
  4. additionwas added to the residue
  5. customThe resulting solid was collected
  6. washwashed with water
  7. customdried
  8. customrecrystallised from IMS