関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,8-Dinitro-9,10-anthraquinone | HCID 67210 | — |
| 反応物 | Sodium sulfide nonahydrate | HCID 73972 | — |
| 反応物 | 1,8-Bis(chloroacetamido)anthraquinone | HCID 46928041 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,8-Diamino-9,10-anthracenedione | HCID 8511 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08053583B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-41fb87150f0247df9b854dce5420b4c7 |
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| 出典メモ | uspto-grants-2011_11 |
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