HRID884993

反应详情

EQUATION

反应方程式

HRID 884993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.7 g of 3-ethyl isonicotinonitrile, 1.63 g of sodium hydroxide, 20 ml of ethanol and 20 ml of water was heated to reflux for five hours. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. 3 M hydrochloric acid was added so that pH of the resultant residue became about 3, which was concentrated under reduced pressure again. To the resultant solid, 50 ml of ethanol was added and heated to reflux for five minutes, followed by hot filtration. To the solid collected by filtration, the same operation was carried out by using 50 ml each of ethanol. Combined filtrates were concentrated to give 2.49 g of 3-ethyl isonicotinic acid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for five hours
  3. concentrationconcentrated under reduced pressure
  4. addition3 M hydrochloric acid was added so that pH of the resultant residue
  5. concentrationwas concentrated under reduced pressure again
  6. additionTo the resultant solid, 50 ml of ethanol was added
  7. temperatureheated
  8. temperatureto reflux for five minutes
  9. filtrationfollowed by hot filtration
  10. filtrationTo the solid collected by filtration
  11. concentrationCombined filtrates were concentrated