HRID67949

反应详情

EQUATION

反应方程式

HRID 67949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4.14 g (0.18 g. atom) of sodium in 100 ml. of ethanol was added 28.8 g. (0.18 mole) of diethyl malonate. After stirring at room temperature for 5 minutes, 7.14 g. (0.06 mole) of 2-aminonicotinonitrile was added and the mixture was heated under reflux for 6 hours. The mixture was cooled and was diluted with 100 ml. of water and was acidified with conc. hydrochloric acid. On cooling, a precipitate was formed which was collected and was triturated with 1000 ml. of boiling ethanol. The mixture was filtered and the filtrate was cooled in ice to precipitate 2.9 g. of product, m.p. 264°-267° C. dec.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 6 hours
  3. temperatureThe mixture was cooled
  4. additionwas diluted with 100 ml
  5. temperatureOn cooling
  6. customa precipitate was formed which
  7. customwas collected
  8. customwas triturated with 1000 ml
  9. filtrationThe mixture was filtered
  10. temperaturethe filtrate was cooled in ice
  11. customto precipitate 2.9 g