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2-Fluoro-5-methylbenzonitrile → N-(2-Cyano-4-methylphenyl)-4-piperidone propylene ketal
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Fluoro-5-methylbenzonitrile | HCID 2774584 | — |
| 反応物 | 4-Piperidone propylene ketal | HCID 12954117 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium Carbonate | HCID 10340 | — |
| 生成物 | N-(2-Cyano-4-methylphenyl)-4-piperidone propylene ketal | HCID 86757963 | — |
反応手順
A solution of 2-fluoro-5-methylbenzonitrile (2.76 g, 20.4 mmol) and 4-piperidone propylene ketal (3.39 g, 21.5 mmol) in DMF (50 mL) was heated in an oil bath (90° C., 20 h). The mixture was diluted with ether and sodium carbonate solution. The aqueous layer was extracted with two additional portions of ether and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. PCTLC (SiO2, 6 mm, 50-0% hexane/CHCl3) afforded the title compound (29).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06376503B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-2ca31ef732be4aaaa27a5267183f06eb |
| 出典メモ | uspto-grants-2002_04 |