HRID372210
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
PROCEDURE
实验过程
A solution of 10.1 g (0.05 mole) of methyl 2-methoxy-6-chloronicotinate in 20 ml of methanol is added dropwise at 70° C in the course of 30 minutes to 500 ml of 0.1 N aqueous sodium hydroxide solution. After completion of the addition, the mixture is refluxed for 1 hour. The clear solution is concentrated in vacuo to approx. 100 ml and acidified with 2 N hydrochloric acid to pH 3. The precipitate which has formed is collected by filtration, washed with a small amount of water and dried. The residue is recrystallized from benzene-petroleum ether to yield pure 2-methoxy-6-chloronicotinic acid with a melting point of 210°-215° C.
WORKUP
后处理
- additionAfter completion of the addition
- temperaturethe mixture is refluxed for 1 hour
- concentrationThe clear solution is concentrated in vacuo to approx. 100 ml
- customThe precipitate which has formed
- filtrationis collected by filtration
- washwashed with a small amount of water
- customdried
- customThe residue is recrystallized from benzene-petroleum ether