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Acetic Acid → 2-Methyl-4-piperidinone acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 1-Benzyl-2-methylpiperidin-4-one | HCID 11095707 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | 2-Methyl-4-piperidinone acetate | HCID 66684542 | 99% |
反応手順
To a solution of the product of step B (3.8 g, 18.7 mmol) in acetic acid (20 mL) was added Pd/C 10% (380 mg) cautiously. The resulting mixture was hydrogenated at 50 psi H2 for 3 h. The reaction mixture was filtered through celite and washed with acetic acid (20 mL). The filtrate was concentrated in vacuo to yield 2-methylpiperidin-4-one acetate as a brown oil (2.98 g, >99%) which was sufficiently pure for the next step: 1H NMR (CD3OD, 400 MHz) δ 3.24-3.19 (m, 1H), 2.86-2.81 (m, 1H), 2.74-2.67 (m, 1H), 2.51-2.49 (m, 2H), 2.37-2.28 (m, 2H), 2.22-2.18 (m, 1H), 2.12-2.02 (m, 2H), 1.08 (d, J=6.4 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09067949B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-e1c68e2827b44da0962e2bcf4acbee36 |
| 出典メモ | uspto-grants-2015_06 |