HRID430560

反应详情

EQUATION

反应方程式

HRID 430560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

under a nitrogen atmosphere, 3-fluoroaniline (50.0 g, 0.45 mol) and diethyl ethoxymethylmalonate (91 mL, 0.45 mol) were combined and heated at 100° C. for 3 hours. The reaction was allowed to cool to ambient temperature and it solidified. Dowtherm A (200 mL) was added and the reaction mixture was heated at 240° C. for 4 hours. The reaction mixture was allowed to cool to ambient temperature. The resulting precipitate was isolated by filtration, washed with hexane and then dried in a vacuum oven to provide 71.5 g of ethyl 7-fluoro-4-hydroxy-3-quinolinecarboxylate.

WORKUP

后处理

  1. temperatureto cool to ambient temperature
  2. temperaturethe reaction mixture was heated at 240° C. for 4 hours
  3. temperatureto cool to ambient temperature
  4. customThe resulting precipitate was isolated by filtration
  5. washwashed with hexane
  6. customdried in a vacuum oven