関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(Pyridin-3-yl)ethan-1-amine | HCID 2771688 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 6,4'-Dimethoxybiphenyl-3-carbaldehyde | HCID 22391191 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | (6,4'-Dimethoxy-biphenyl-3-ylmethyl)-(1-pyridin-3-yl-ethyl)amine | HCID 22391323 | 50% |
反応手順
1-Pyridin-3-yl-ethylamine (245 mg, 2 mmol) and 6,4′-Dimethoxy-biphenyl-3-carbaldehyde (121 mg, 0.5 mmol) were dissolved in dichloroethane (10 mL). After stirring for 6 h at room temperature, the sodium triacetoxyborohydride (212 mg, 1.0 mmol, Aldrich) was added to the solution at 0 C. The mixture was stirred under nitrogen at room temperature for overnight then the reaction was cooled at ice bath and quenched with saturated aqueous sodium bicarbonate (10 mL). The organic phase was separated and the aqueous phase was extracted with dichloroethane (10 mL×3). The combined organic layers were dried over anhydrous magnesium sulfate and concentrated via vacuo. The crude was purified by column chromatography (silica gel, ethyl acetate) to give the title compound as white solid in 50% yield (87 mg, 0.25 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07196102B2 |
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| 出典データセット | uspto-grants-2007_03 |
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| ORD ID | ord-6eb08a0910f14b3eac3200d70a650fab |
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| 出典メモ | uspto-grants-2007_03 |
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