関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylazanium;chloride | HCID 11649 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 1-(3-(Benzyloxy)-6-bromopyridin-2-yl)ethanone | HCID 86662736 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(6-Bromo-3-hydroxypyridin-2-YL)ethanone | HCID 72218015 | 83% |
反応手順
To a suspension (30 mL) of aluminum chloride (3.96 g) in toluene was added trimethylammonium chloride (1.32 g), and the mixture was stirred under argon atmosphere at room temperature for 1 hr. A solution (30 mL) of 1-[3-(benzyloxy)-6-bromopyridin-2-yl]ethanone (2.81 g) synthesized above in toluene was added to the mixture, and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated under reduced pressure, saturated aqueous Rochelle salt solution was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane) to give the title object compound (1.64 g, 83%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08436043B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-a2661d90993c45eda2e624fbe304906a |
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| 出典メモ | uspto-grants-2013_05 |
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