反应 #2320171

反应方程式

NaOH

4-bromo-6-methoxy-[1,5]naphthyridine-3-carboxylic acid ethyl ester

HCl

→

title compound

4-Bromo-6-methoxy-[1,5]naphthyridine-3-carboxylic acid

溶剂

THF

反应条件

后处理

1. 1
   其他the THF was removed in vacuo
2. 2
   workup.ADDITION2 N HCl was added to pH 2
3. 3
   workup.ADDITIONwater (250 mL) was added
4. 4
   温度the mixture was cooled thoroughly in ice
5. 5
   过滤The solid was collected by suction filtration
6. 6
   洗涤washed with water
7. 7
   其他dried (
8. 8
   其他a rotary evaporator at 50° C.

实验过程

2 N NaOH (300 mL, 600 mmol) was added dropwise over 30 min to a stirred solution of 4-bromo-6-methoxy-[1,5]naphthyridine-3-carboxylic acid ethyl ester (83.56 g, 268 mmol) in THF (835 mL). Stirring was continued overnight, at which time LC/MS showed that the saponification was complete. 2 N HCl was added to pH 6 and the THF was removed in vacuo. 2 N HCl was added to pH 2, then water (250 mL) was added, and the mixture was cooled thoroughly in ice. The solid was collected by suction filtration, washed with water and dried (first using a rotary evaporator at 50° C. and then under high vacuum at 50° C. overnight) to give the title compound (76.7 g, slightly over quantitative). This material was used without further purification.

来源