関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | 9,10-Anthracenedione, 1-amino-2,4-dichloro- | HCID 72910 | — |
| 反応物 | Sulfuric acid hydrate (1:1) | HCID 21910475 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 9,10-Anthracenedione, 1-amino-2-chloro-4-hydroxy- | HCID 75590 | 95% |
反応手順
A stirred reactor is charged with 184 parts of sulfuric acid monohydrate and 4.8 parts (1 equivalent) of paraformaldehyde are added, with stirring, over about 15 minutes. Stirring is continued until a solution is obtained. This solution is then heated to 60°-65° C. and 46.5 parts of 98% 1-amino-2,4-dichloroanthraquinone are added. The reaction mixture is heated for 1 hour to 110° C. and this temperature is maintained for 3 hours. The mixture is cooled to 100° C. and 870 parts of water are added. The resultant suspension is heated to 90°-95° C. and stirred for 2 hours at this temperature, then cooled and filtered. The filter cake is washed with hot water and the product is dried in vacuo at 80°-90° C., affording 43.3 parts (95% yield) of 1-amino-2-chloro-4-hydroxyanthraquinone. Rf =0.29 (eluant: concentrated formic acid, saturated with 1-bromonaphthalene).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04657707 |
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| 出典データセット | uspto-grants-1987_04 |
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| ORD ID | ord-6c9e49b6536740b6a68ca3ef82e0330e |
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| 出典メモ | uspto-grants-1987_04 |
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