盐酸 → HCID 178507708，化合物

HRID 463562笔记

反应方程式

HRID 463562 反应方程式
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]

参与物

8

反应物 6

HCID 313盐酸HCID 1118四氧化硫HCID 6710氨基蒽醌HCID 214021,4-二氨基蒽-9,10-二醇HCID 24526Chlorine2 次HCID 5462222钾

产物 1

HCID 178507708HCID 178507708，化合物收率 103.5%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-a4965a70162f4f74b2e6d5f87878b374
来源数据集
uspto-grants-1985_05
专利号
US04520202

反应笔记

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