1-Chloroanthraquinone → Anthrimide

HRID 542992

反応式

HRID 542992 の反応式
Cl[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[CH:5]=[CH:4][CH:3]=1.[NH2:18][C:19]1[C:32]2[C:31](=[O:33])[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[C:24](=[O:34])[C:23]=2[CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+].[N+](C1C=CC=CC=1)([O-])=O>[Cu]Cl>[CH:10]1[CH:9]=[C:8]2[C:7]([C:6]3[CH:5]=[CH:4][CH:3]=[C:2]([NH:18][C:19]4[C:32]5[C:31]([C:30]6[C:25]([C:24](=[O:34])[C:23]=5[CH:22]=[CH:21][CH:20]=4)=[CH:26][CH:27]=[CH:28][CH:29]=6)=[O:33])[C:15]=3[C:14](=[O:16])[C:13]2=[CH:12][CH:11]=1)=[O:17]

参加物

6

反応物 4

HCID 67091-ChloroanthraquinoneHCID 67101-AminoanthraquinoneHCID 7416NitrobenzeneHCID 10340Sodium Carbonate

生成物 1

HCID 6700Anthrimide

試薬・触媒・溶媒 1

HCID 62652Cuprous chloride触媒2 回

反応条件

温度
190 °C

実験手順

66 parts of 1-chloroanthraquinone, 60.5 parts of 1-aminoanthraquinone, 26.4 parts of sodium carbonate and 0.75 part of copper(I) chloride are suspended in 550 parts of nitrobenzene. With stirring, the mixture is heated to 190° C. and then a further 0.75 part of copper(I) chloride is added. The reaction mixture is heated to 206° C. and stirred for 3 hours at this temperature while distilling off the water of reaction. The batch is then heated to 214° C. and the pressure rises to about 1 bar. Stirring is continued for another 2 hours under these conditions. The reaction mixture is then cooled slightly and the nitrobenzene is removed by distillation. After drying there are obtained about 115 parts of anthrimide, which is suitable for further processing to give vat dyes.

後処理

  1. temperatureThe reaction mixture is heated to 206° C.
  2. stirringstirred for 3 hours at this temperature
  3. distillationwhile distilling off
  4. customthe water of reaction
  5. temperatureThe batch is then heated to 214° C.
  6. stirringStirring
  7. temperatureThe reaction mixture is then cooled slightly
  8. customthe nitrobenzene is removed by distillation
  9. customAfter drying there

出典と根拠

ORDレコード
ord-9c2fec673e5f4601a85c0970a6f0fdfc
出典データセット
uspto-grants-1987_04
特許番号
US04659831

関連ノート

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