関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyric Acid | HCID 264 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2,6-Diamino-3-nitropyridine | HCID 319998 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | 5-Butyramido-2-propylimidazo[4,5-b]pyridine | HCID 22407381 | 49.1% |
反応手順
A mixture of 2,6-diamino-3-nitropyridine (878 mg, 5.7 mmol) and Pd-C (10%, 100 mg) in MeOH (100 mL) was stirred under 1 atm. H2 for 16 hours. The mixture (containing the air sensitive triamine) was filtered, evaporated, and to this flask was added polyphosphoric acid (15 mL) and butyric acid (1.05 mL, 11.5 mmol). This mixture was heated to 80° C. for 5 hours, cooled to room temperature, diluted with water and neutralized with concentrated NH4OH. Extractive workup (CH2Cl2) gave 345 mg of 5-(butyramido)-2-propylimidazo[4,5-b]pyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05157026 |
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| 出典データセット | uspto-grants-1992_10 |
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| ORD ID | ord-456bbe93220848599009a8d9c9554856 |
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| 出典メモ | uspto-grants-1992_10 |
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