1-Aminoanthraquinone → HCID 178507708、化合物

HRID 1262492ノート

反応式

HRID 1262492 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.[NH2:19][C:20]1[C:33]2[C:32](=[O:34])[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:25](=[O:35])[C:24]=2[CH:23]=[CH:22][CH:21]=1.[K].OS([O-])=O.[Na+]>OS(O)(=O)=O.O>[CH:10]1[CH:9]=[C:8]2[C:7]([C:6]3[C:15]([C:14](=[O:16])[C:13]2=[CH:12][CH:11]=1)=[C:2]([NH:1][C:23]1[CH:22]=[CH:21][C:20]([NH2:19])=[C:33]2[C:32]([C:31]4[C:26]([C:25](=[O:35])[C:24]=12)=[CH:27][CH:28]=[CH:29][CH:30]=4)=[O:34])[CH:3]=[CH:4][C:5]=3[NH2:18])=[O:17]

参加物

7

反応物 4

HCID 67101-AminoanthraquinoneHCID 31420Disperse Violet 1HCID 5462222PotassiumHCID 23665763Sodium Bisulfite

生成物 1

HCID 178507708HCID 178507708、化合物収率 100.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 1118Sulfuric Acid溶媒

反応条件

温度
15 °C

実験手順

52.0 g of 1,4-diaminoanthraquinone (92% pure) and 47.0 g of 1-aminoanthraquinone (98% pure) are dissolved in 512 g of 96% strength H2SO4 and this solution is added dropwise, with efficient stirring, to 460 g of water within 30 minutes. After cooling to about 15° C., 110.0 g of potassium peroxodisulphate are added, with efficient stirring, within about 3 hours and the mixture is allowed to warm slowly to 20° C. The melt is stirred at about 20° C. for 2-3 hours and then added to a mixture of 600 ml of water and 150 ml of 40% strength NaHSO3 solution and, after addition of a defoamer, the mixture is heated to 80°-90° C. in 30 minutes. After 30 minutes at 80°-90° C., the solid is filtered off hot with suction, washed with water to neutrality and dried at 100° C. 97.4 g of 4,4'-diamino-1,1'-dianthrimide (81% pure), corresponding to 86% of theory, were obtained.

後処理

  1. temperatureto warm slowly to 20° C
  2. additionafter addition of a defoamer
  3. temperaturethe mixture is heated to 80°-90° C. in 30 minutes
  4. waitAfter 30 minutes at 80°-90° C.
  5. filtrationthe solid is filtered off hot with suction
  6. washwashed with water to neutrality
  7. customdried at 100° C

出典と根拠

ORDレコード
ord-ae5b2911669a448cb3633f1c92241e00
出典データセット
uspto-grants-1984_06
特許番号
US04452742

反応ノート

読み込み中…