関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 反応物 | 1,3-Di(2-pyridyl)-1,3-propanedione | HCID 2728494 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Amino-4-(2-pyridyl)thiazol-5-yl 2-pyridyl ketone | HCID 23144668 | 51% |
反応手順
1,3-Di(2-pyridyl)propane-1,3-dione (1.17 g, 5.15 mmol) was dissolved in acetic acid (20 mL), and bromine (856 mg, 5.35 mmol) was added thereto, followed by stirring at 80° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, and the resulting residue was suspended in ethanol (30 mL), and triethylamine (0.750 mL, 5.38 mmol) and thiourea (416 mg, 5.47 mmol) were added thereto, followed by stirring under heating and reflux for 30 minutes. Aqueous saturated sodium hydrogencarbonate solution was added to the reaction mixture, followed by extraction with chloroform. The solvent was distilled away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (chloroform:methanol=9:1) to afford the entitled Compound 630 (739 mg, 51%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07880013B2 |
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| 出典データセット | uspto-grants-2011_02 |
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| ORD ID | ord-b756ff4b5d4e4898a65002674cedb26d |
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| 出典メモ | uspto-grants-2011_02 |
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