関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N'-(5-bromopyridin-2-yl)-2,2,2-trifluoroacetohydrazide | HCID 54363377 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Bromo-3-(trifluoromethyl)-(1,2,4)triazolo(4,3-a)pyridine | HCID 58118906 | 78.1% |
反応手順
A mixture of polyphosphoric acid (20 mL, 175 mmol) and N′-(5-bromopyridin-2-yl)-2,2,2-trifluoroacetohydrazide (1.9 g, 6.69 mmol) was stirred at 120° C. for 20 hours and then poured in to water. The mixture was then basified with saturated aqueous sodium bicarbonate solution and extracted with dichloromethane (3×250 mL). The organic phases were combined and washed with brine (1×100 mL), dried with MgSO4 and evaporated to give an involatile residue. The residue was purified by flash chromatography on silica-gel using an increasing gradient of ethyl acetate in isohexane as eluant to give 6-bromo-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridine (1.39 g, 78%) as a beige solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08003649B2 |
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| 出典データセット | uspto-grants-2011_08 |
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| ORD ID | ord-f7a05e46965e4096ac6452a06daf1ade |
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| 出典メモ | uspto-grants-2011_08 |
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