HRID639624

反应详情

EQUATION

反应方程式

HRID 639624 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

2,4-Dihydroxy-6-trifluoromethyl-nicotinic acid ethyl ester (62 g/247 mmols) was added in several portions over 30 mins to 6M HCl(aq) (620 mls) at reflux. The resulting mixture was then heated at 100° C. overnight with vigorous stirring to obtain complete solution. The solution was then allowed to cool and concentrated in vacuo to a white solid. This was slurried in water (250 mls) and adjusted to pH 7 with conc. ammonia to get heavy white suspension. The resulting solid was collected by filtration, rinsed through with fresh water, and dried to provide the title compound (44.0 g) as a white solid.

WORKUP

后处理

  1. temperatureat reflux
  2. customto obtain complete solution
  3. temperatureto cool
  4. concentrationconcentrated in vacuo to a white solid
  5. customto get heavy white suspension
  6. filtrationThe resulting solid was collected by filtration
  7. washrinsed through with fresh water
  8. customdried