Sodium Hydroxide → 1,8-Diamino-9,10-anthracenedione

HRID 556196

反応式

HRID 556196 の反応式
ClCC([NH:5][C:6]1[C:19]2[C:18](=[O:20])[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][C:16]=3[NH:21]C(=O)CCl)[C:11](=[O:26])[C:10]=2[CH:9]=[CH:8][CH:7]=1)=O.[N+](C1C2C(=O)C3C(=CC=CC=3[N+]([O-])=O)C(=O)C=2C=CC=1)([O-])=O.O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+].[OH-].[Na+]>C(O)C>[NH2:5][C:6]1[C:19]2[C:18](=[O:20])[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][C:16]=3[NH2:21])[C:11](=[O:26])[C:10]=2[CH:9]=[CH:8][CH:7]=1

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 672101,8-Dinitro-9,10-anthraquinoneHCID 73972Sodium sulfide nonahydrateHCID 469280411,8-Bis(chloroacetamido)anthraquinone

生成物 1

HCID 85111,8-Diamino-9,10-anthracenedione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In the step S1, a manufacturing method of 1,8-bis(chloroacetamido)anthraquinone includes the steps of: add 1,8-dinitroanthraquinone with ethanol, and then add sodium sulfide nonahydrate and sodium hydroxide solution into the mixture to be mixed and reflux heated. After standing and filtration, 1,8-diaminoanthraquinone is obtained by recrystallization of the solution. Next the 1,8-diaminoanthraquinone is dissolved in N,N-dimethylform amide, and pyridine is added for catalyzing, and then chloroacetyl chloride is added into and mixed with the mixture to react. Pour the solution into ice water, 1,8-bis(chloroacetamido) anthraquinone is obtained after filtration and recrystallization of the solution. The step of adding pyridine for catalyzing is run under an ice-bath while in the step of adding and mixing chloroacetyl chloride into the mixture, the ice bath is removed, the nitrogen gas is introduce and the step is run under light protection condition. The step of adding and mixing chloroacetyl chloride into the mixture is run at the room temperature for 24 hours.

後処理

  1. temperaturereflux
  2. temperatureheated
  3. filtrationfiltration

出典と根拠

ORDレコード
ord-41fb87150f0247df9b854dce5420b4c7
出典データセット
uspto-grants-2011_11
特許番号
US08053583B2

関連ノート

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