HRID249288

反应详情

EQUATION

反应方程式

HRID 249288 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6,7-Difluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid ethyl ester (10.0 g, 39.5 mmol), 1-bromo-2-fluoroethane (25.1 g, 197.5 mmol) and potassium carbonate (10.9 g, 79 mmol) were combined in dimethylformamide (200 ml) and heated to 90° for 20 hours. The reaction mixture was poured into cold water (1.5 l), and the copious precipitate was filtered. The precipitate was washed with cold water and recrystallized from ethyl acetate to provide the title product as light brown needles, m.p. 178°-180° (8.22 g, 27.5 mmol, 70% yield).

WORKUP

后处理

  1. temperatureheated to 90° for 20 hours
  2. filtrationthe copious precipitate was filtered
  3. washThe precipitate was washed with cold water
  4. customrecrystallized from ethyl acetate