関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nipecotic Acid | HCID 4498 | — |
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 21041140 | HCID 21041140 | 44.9% |
反応手順
To a solution added of nipecotic acid (8.0 g, 61.9 mmol) in N,N-dimethylformamide (80 mL) is benzyl bromide (31.8 g, 186 mmol) and potassium carbonate (42.8 g, 310 mmol). The mixture is heated at 70° C. for 18 hours and diluted with ethyl acetate and water. The organic extract is washed with 1.0 M hydrochloric acid, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue is purified by column chromatography (1:7 ethyl acetate/hexanes) to afford the title compound (8.6 g). 1H NMR (200 MHz, DMSO-d6): δ 7.27–7.42 (m, 10H), 5.07 (s, 2H), 3.45 (s, 2H), 2.88–2.49 (m, 3H), 2.32–1.32 (m, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094780B1 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-d2eb413225c145a683f8e6c5e0750cba |
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| 出典メモ | uspto-grants-2006_08 |
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