関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Amino-4-bromopyridine | HCID 693282 | — |
| 反応物 | (2-Methoxypyridin-3-yl)boronic acid | HCID 2762709 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Methoxy-[3,4'-bipyridin]-2'-amine | HCID 50957286 | 93.9% |
反応手順
To 4-bromopyridin-2-amine (0.5 g, 2.8 mmol), 2-methoxypyridin-3-ylboronic acid (0.52 g, 3.4 mmol) in DMF (25 mL) was added 1N sodium carbonate (10 mL, 2.3 mmol), followed by 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex (0.21 g, 0.26 mmol). The reaction mixture was stirred for 3 hours at 85° C. and then cooled to room temperature. The product was extracted with ethyl acetate (2×50 mL), dried with MgSO4, filtered, and concentrated in vacuo. The crude product was purified by chromotography (Biotage: 100 to 90/10% ethyl acetate-ethyl acetate/methanol) to yield 2-methoxy-3,4′-bipyridin-2′-amine (0.53 g, 2.63 mmol, 93% yield) as a brown powder. The product was taken directly to the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07863291B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-a3e2247148e14db7a13681de1b3ce2c7 |
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| 出典メモ | uspto-grants-2011_01 |
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