反応 #54213

反応方程式

disodiumdimercaptomethylene malononitrile

DMF

water

→

4,5-Dihydro-4-oxo-1,3-dithiolo (4,5-d)-pyridazine-2-ylidene-propanedinitrile

収率 90.0%

反応条件

後処理

1. 1
   workup.ADDITIONwas added 16.5 g (0.1 mole) of 4,5-dichloro-3-pyridiazone
2. 2
   workup.ADDITIONwas thereafter poured
3. 3
   workup.WAITto stand for four hours during which time
4. 4
   その他a yellow-gray precipitate slowly formed
5. 5
   その他This precipitate was separated by filtration
6. 6
   洗浄washed with water
7. 7
   その他dried in vacuo
8. 8
   その他to yield 21.1 g (90% yield from the pyridiazone) of a yellow-gray solid, m.p. (decomposition) 310°-340° C.

実験手順

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.

出典