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

HRID 556196

반응식

HRID 556196 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  1. temperaturereflux
  2. temperatureheated
  3. filtrationfiltration

출처 및 근거

ORD 기록
ord-41fb87150f0247df9b854dce5420b4c7
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053583B2

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