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Dimethylformamide → 3-Allyl-1,3-dimethyl-piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Allyl bromide | HCID 7841 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,3-Dimethyl-4-piperidone | HCID 107311 | — |
| 生成物 | 3-Allyl-1,3-dimethyl-piperidin-4-one | HCID 13740022 | — |
反応手順
1,3-Dimethyl-piperidin-4-one (6 g, 47.24 mmol) was dissolved in 20 mL DMF and sodium hydride (2.07 g, 51.95 mmol) was added portionwise at 0° C. under nitrogen atmosphere. This was followed by dropwise addition of allyl bromide (5.71 g, 47.19 mmol) in 4 mL DMF at 0° C. under nitrogen atmosphere. The reaction mixture was stirred at RT for 15 min, quenched with ice-water and extracted with EtOAc (3×100 mL), The organic layer was washed with water (3×100 mL), dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 100-200 mesh) eluting with 7% EtOAc in hexane to obtain 3.2 g of 3-allyl-1,3-dimethyl-piperidin-4-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09040519B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-1aa482f18b2844deb63dd93ae21ad295 |
| 出典メモ | uspto-grants-2015_05 |