反応 #54681

反応方程式

disodiumdimercaptomaleonitrile

water

→

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

収率 43.0%

溶媒

DMF

反応条件

後処理

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

実験手順

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.

出典