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

HRID 26403ノート

反応式

HRID 26403 の反応式
[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

参加物

4

反応物 2

HCID 962WaterHCID 56924615DISODIUM DIMERCAPTOMALEONITRILE

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
20 °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.

後処理

  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.

出典と根拠

ORDレコード
ord-004f8f7d166246c6b337059c1d1d927f
出典データセット
uspto-grants-1979_04
特許番号
US04150130

反応ノート

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