Hydrochloric Acid → HCID 178507708、化合物

HRID 463562ノート

反応式

HRID 463562 の反応式
ClCl.[CH:3]1[CH:8]=[C:7]2[C:9]([OH:20])=[C:10]3[C:15](=[C:16]([OH:17])[C:6]2=[CH:5][CH:4]=1)[C:14]([NH2:18])=[CH:13][CH:12]=[C:11]3[NH2:19].OS(O)(=O)=O.Cl.[NH2:27][C:28]1[C:41]2[C:40](=[O:42])[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[C:33](=[O:43])[C:32]=2[CH:31]=[CH:30][CH:29]=1.[K]>O>[CH:3]1[CH:8]=[C:7]2[C:9]([C:10]3[C:15]([C:16](=[O:17])[C:6]2=[CH:5][CH:4]=1)=[C:14]([NH:18][C:31]1[CH:30]=[CH:29][C:28]([NH2:27])=[C:41]2[C:40]([C:39]4[C:34]([C:33](=[O:43])[C:32]=12)=[CH:35][CH:36]=[CH:37][CH:38]=4)=[O:42])[CH:13]=[CH:12][C:11]=3[NH2:19])=[O:20]

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 67101-AminoanthraquinoneHCID 214029,10-Anthracenediol, 1,4-diamino-HCID 24526Chlorine2 回HCID 5462222Potassium

生成物 1

HCID 178507708HCID 178507708、化合物収率 103.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Chlorine is passed at 100° C. into a solution of 52.0 g of leuco-1,4-diaminoanthraquinone (94%) in 410 g of 96% strength H2SO4 until the leuco compound has just disappeared. Excess chlorine as well as hydrogen chloride is expelled by means of air. The batch is then allowed to cool down to room temperature, during which time 48.0 g of 1-aminoanthraquinone (98%) are added, and the mixture is then added dropwise to 410 g of water. 95.0 g of potassium peroxodisulphate are added in portions in the course of about 1 hour at 40°-50° C. to the paste. Stirring is allowed to continue for about 30 minutes at 30°-50° C., and the solids are filtered off with suction and washed with water until almost neutral. The press cake is washed with 300 ml of 10% strength NaHSO3 solution, and then with water, and dried at 100° C. 102.3 g of 4,4'-diamino-1,1'-dianthrimide (79% pure) are obtained; this result corresponds to 87% of theory.

後処理

  1. additionare added
  2. filtrationthe solids are filtered off with suction
  3. washwashed with water until almost neutral
  4. washThe press cake is washed with 300 ml of 10% strength NaHSO3 solution
  5. dry with materialwith water, and dried at 100° C

出典と根拠

ORDレコード
ord-a4965a70162f4f74b2e6d5f87878b374
出典データセット
uspto-grants-1985_05
特許番号
US04520202

反応ノート

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