Dimethyl Sulfoxide → 2,3-Anthracenedicarbonitrile, 1,4-diamino-9,10-dihydro-9,10-dioxo-

HRID 441769

反応式

HRID 441769 の反応式
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]([NH2:18])=[CH:4][CH:3]=1.CS(C)=O.[C-:23]#[N:24].[Na+].[Cl-].[NH4+:27].[CH3:28]O>>[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[C:5]([NH2:18])=[C:4]([C:23]#[N:24])[C:3]=1[C:28]#[N:27]

参加物

6

反応物 5

HCID 679Dimethyl SulfoxideHCID 887MethanolHCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 31420Disperse Violet 1

生成物 1

HCID 664772,3-Anthracenedicarbonitrile, 1,4-diamino-9,10-dihydro-9,10-dioxo-

実験手順

A suspension of 10 parts of 1,4-diaminoanthraquinone in 90 parts of dimethylsulfoxide is heated to 120° to 125° C., 12.5 parts of sodium cyanide is added all at once and then 5 parts of ammonium chloride is added within 15 minutes under an effective fume hood. The whole is stirred for another 3 hours at 120° to 125° C., whereupon one makes sure by a chromatogram that practically all of the starting material has been used up. The reaction mixture is allowed to cool and is diluted with 300 parts by volume of cold methanol, air is blown through under an effective fume hood for a short period, the precipitate is suction filtered and the filter cake is washed with methanol until the liquid running away is almost colorless. After drying, 9.5 parts of 1,4-diaminoanthraquinone-2,3-dinitrile is obtained.

後処理

  1. temperatureis heated to 120° to 125° C.
  2. additionis added within 15 minutes under an effective fume hood
  3. temperatureto cool
  4. waitis blown through under an effective fume hood for a short period
  5. filtrationfiltered
  6. washthe filter cake is washed with methanol until the liquid
  7. customAfter drying

出典と根拠

ORDレコード
ord-860ac5cb959f4fe692b9aebd91aba7c5
出典データセット
uspto-grants-1977_08
特許番号
US04042605

関連ノート

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