関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,7,9-Trimethyl 4,5-dihydro-4,5-dioxo-1H-pyrrolo(2,3-f)quinoline-2,7,9-tricarboxylate | HCID 451469 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Pyrroloquinoline Quinone | HCID 1024 | — |
反応手順
To a solution of potassium carbonate (about 439 g, 3.18 mol) in water (about 4.5 L), 4,5-dioxo-4,5-dihydro-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic acid trimethyl ester (about 200 g, 0.53 mol) is added at about 25° C. The reaction mixture is allowed to stir at about 80° C. over a period of about 12 hours. Completion of reaction is monitored by HPLC. Thereafter, the reaction mixture is acidified (pH: 2.0) with 1N hydrochloric acid to precipitate the product [4,5-Dioxo-4,5-dihydro-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic acid] as dark red solid (about 160 g, 91%). 1H NMR (DMSO-d6, 300 MHz): 7.21 (s, 1H), 8.60 (s, 1H), 13.42 (s, 1H); LC-MS (ESI): 329 (M-H), Purity by HPLC: 98%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115128B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-e6057860efef4aeabb53cc17c6cff7bc |
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| 出典メモ | uspto-grants-2015_08 |
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