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

HRID 26403노트

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HRID 26403 반응식
[SH:1]/[C:2](/[C:7]#[N:8])=[C:3](\[SH:6])/[C:4]#[N:5].[Na].[Na].[OH2:11]>CN(C=O)C>[O:11]=[C:4]1[NH:5][N:8]=[CH:7][C:2]2[S:1][C:2]([C:7]#[N:8])=[C:3]([C:4]#[N:5])[S:6][C:3]1=2

참가 물질

4

반응물 2

HCID 962WaterHCID 56924615DISODIUM DIMERCAPTOMALEONITRILE

생성물 1

HCID 189912865,6-Dihydro-5-oxo-1,4-dithiino(2,3-d)-pyridazine-2,3-dicarbonitrile수율 43%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
20 °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.

후처리

  1. additionwas thereafter poured
  2. waitto stand for four hours during which time
  3. customa brown precipitate slowly formed
  4. customThis precipitate was separated by filtration
  5. washwashed with water
  6. customdried in vacuo
  7. customto yield 10.2 g (43% yield from the pyridiazone) of a brown solid, m.p. (decomposition) 240°-260° C.

출처 및 근거

ORD 기록
ord-004f8f7d166246c6b337059c1d1d927f
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150130

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