化工社化工社 化学情報印刷レポート · 研究参考用
1-Methylimidazole → 1-(3-Chloro-4-fluorophenyl)propan-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Methylimidazole | HCID 1390 | — |
| 反応物 | 2-(3-Chloro-4-fluorophenyl)acetic acid | HCID 2773721 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 1-(3-Chloro-4-fluorophenyl)propan-2-one | HCID 55273566 | 79% |
反応手順
To a solution of 2-(3-chloro-4-fluorophenyl)acetic acid (18.46 g, 97.89 mmol) in acetic anhydride (463 mL) was added N-methylimidazole (3.9 mL) and the reaction mixture was stirred overnight at room temperature. The reaction mixture was partitioned between ethyl acetate and saturated sodium bicarbonate solution and organic layer was concentrated and purified by flash column chromatography (silica gel, ethyl acetate/hexanes) to give a colorless oil (14.5 g, 79%). 1H NMR (400 MHz, CDCl3) δ 7.23 (dd, J=6.9, 2.1 Hz, 1H), 7.14-7.00 (m, 2H), 3.66 (s, 2H), 2.19 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09102614B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-6c2c69c9e4604669bf78354308ba7cf5 |
| 出典メモ | uspto-grants-2015_08 |