HRID639624
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux
- customto obtain complete solution
- temperatureto cool
- concentrationconcentrated in vacuo to a white solid
- customto get heavy white suspension
- filtrationThe resulting solid was collected by filtration
- washrinsed through with fresh water
- customdried