HRID372210

反应详情

EQUATION

反应方程式

HRID 372210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionAfter completion of the addition
  2. temperaturethe mixture is refluxed for 1 hour
  3. concentrationThe clear solution is concentrated in vacuo to approx. 100 ml
  4. customThe precipitate which has formed
  5. filtrationis collected by filtration
  6. washwashed with a small amount of water
  7. customdried
  8. customThe residue is recrystallized from benzene-petroleum ether