HRID67949
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
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
- temperaturethe mixture was heated
- temperatureunder reflux for 6 hours
- temperatureThe mixture was cooled
- additionwas diluted with 100 ml
- temperatureOn cooling
- customa precipitate was formed which
- customwas collected
- customwas triturated with 1000 ml
- filtrationThe mixture was filtered
- temperaturethe filtrate was cooled in ice
- customto precipitate 2.9 g