反应详情

温度

20 °C

To a stirred solution of 20 g (0.1 mole) disodiumdimercaptomethylene malononitrile dissolved in 250 ml of DMF was added 16.5 g (0.1 mole) of 4,5-dichloro-3-pyridiazone. The reaction mixture was stirred at room temperature (approximately 20° C.) for 0.25 hours and was thereafter poured with stirring into 1 liter of water. The resulting mixture was allowed to stand for four hours during which time a yellow-gray precipitate slowly formed. This precipitate was separated by filtration, washed with water, and dried in vacuo to yield 21.1 g (90% yield from the pyridiazone) of a yellow-gray solid, m.p. (decomposition) 310°-340° C.

1. additionwas added 16.5 g (0.1 mole) of 4,5-dichloro-3-pyridiazone
2. additionwas thereafter poured
3. waitto stand for four hours during which time
4. customa yellow-gray precipitate slowly formed
5. customThis precipitate was separated by filtration
6. washwashed with water
7. customdried in vacuo
8. customto yield 21.1 g (90% yield from the pyridiazone) of a yellow-gray solid, m.p. (decomposition) 310°-340° C.