Water → 4,5-Dihydro-4-oxo-1,3-dithiolo (4,5-d)-pyridazine-2-ylidene-propanedinitrile
Reaktionsgleichung
[SH:1][C:2](=[C:4]([C:7]#[N:8])[C:5]#[N:6])[SH:3].[Na].[Na].O.C[N:13]([CH:15]=[O:16])C>>[O:16]=[C:15]1[NH:13][N:6]=[CH:5][C:4]2[S:1][C:2](=[C:4]([C:7]#[N:8])[C:5]#[N:6])[S:3][C:2]1=2Komponenten
4
Reaktionsbedingungen
- Temperatur
- 20 °C
Versuchsvorschrift
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.
Aufarbeitung
- additionwas added 16.5 g (0.1 mole) of 4,5-dichloro-3-pyridiazone
- additionwas thereafter poured
- waitto stand for four hours during which time
- customa yellow-gray precipitate slowly formed
- customThis precipitate was separated by filtration
- washwashed with water
- customdried in vacuo
- customto yield 21.1 g (90% yield from the pyridiazone) of a yellow-gray solid, m.p. (decomposition) 310°-340° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-99600fb47d3a49ecb0cdc24f0efcf210
- Quelldatensatz
- uspto-grants-1979_04
- Patentnummer
- US04147784
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