関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Bromocyclobutane | HCID 78110 | — |
| 反応物 | 3-(2-Oxopropyl)benzonitrile | HCID 13354959 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(3-Cyanophenyl)4-cyclobutyl-butan-2-one | HCID 22270763 | — |
反応手順
To a solution of 1.45 g (9.07 mmol) of 1-(3-cyanophenyl)acetone in 18 mL acetonitrile, 1.1 mL (9.5 mmol) cyclobutyl bromide and 5.91 g (18.1 mmol) cesium carbonate were added. After heating the solution in a 60° C. bath overnight, it was cooled and filtered. The filtrate was partitioned between water and EtOAc and the aqueous layer was extracted with EtOAc. The combined organic layer was washed with brine, dried and concentrated. The residue was purified on a flash column using a gradient of 5-10% EtOAc/hexane to isolate the title compound. 1H NMR: (500 MHz, CDCl3): δ 1.5-2.2 (m, 9H), 2.13 (s, 3H), 3.64 (m, 1H), 7.4-7.7 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07423067B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-b35b30713ad8435ca0fdaf1c324a6c9c |
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| 出典メモ | uspto-grants-2008_09 |
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