반응 #54681

반응 방정식

disodiumdimercaptomaleonitrile

water

→

5,6-Dihydro-5-oxo-1,4-dithiino(2,3-d)-pyridazine-2,3-dicarbonitrile

수율 43.0%

용매

DMF

반응 조건

후처리

1. 1
   workup.ADDITIONwas thereafter poured
2. 2
   workup.WAITto stand for four hours during which time
3. 3
   기타a brown precipitate slowly formed
4. 4
   기타This precipitate was separated by filtration
5. 5
   세척washed with water
6. 6
   기타dried in vacuo
7. 7
   기타to yield 10.2 g (43% yield from the pyridiazone) of a brown solid, m.p. (decomposition) 240°-260° C.

실험 절차

To a stirred solution of 20 g (0.1 mole) disodiumdimercaptomaleonitrile 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 1.5 liters of water. The resulting mixture was allowed to stand for four hours during which time a brown precipitate slowly formed. This precipitate was separated by filtration, washed with water, and dried in vacuo to yield 10.2 g (43% yield from the pyridiazone) of a brown solid, m.p. (decomposition) 240°-260° C.

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