HRID249290

反应详情

EQUATION

反应方程式

HRID 249290 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), methyl iodide (56 g, 395 mmol) and potassium carbonate (10.9 g, 79 mmol) were combined in dimethylsformamide and heated to 90° for 20 hours. The reaction mixture was cooled and poured into cold water (1.5 l). The precipitate was filtered, washed with cold water and recrystallized from ethyl acetate to yield the title product as white needles, m.p. 210°-212° (6.60 g, 24.7 mmol, 63% yield).

WORKUP

后处理

  1. temperatureheated to 90° for 20 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationThe precipitate was filtered
  4. washwashed with cold water
  5. customrecrystallized from ethyl acetate