関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Bromomethylcyclopropane | HCID 81503 | — |
| 反応物 | Piperonylamine | HCID 2723901 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(Cyclopropylmethyl)piperidin-4-one | HCID 18002181 | 62% |
反応手順
To a suspension of (bromomethyl)cyclopropane (500 mg, 4 mmol, 1.0 eq.) and 4-piperidone hydrate hydrochloride (579 mg, 4 mmol, 1.0 eq.) in acetonitrile (30 mL) was added sodium carbonate (1.148 g, 11 mmol, 3. eq.). The reaction mixture was stirred 16 h at 85° C. The resulting suspension was filtered and the solid was washed with acetonitrile. The filtrate was concentrated in vacuo and purified by column chromatography on silica eluting with DCM/2N NH3 in methanol 97:3 to yield 339 mg (62%) of the tide compound as yellow oil. MS (m/e): 154.2 (MH+, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07361682B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-a2ae8eef1ddf4083bab3acff954328f8 |
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| 出典メモ | uspto-grants-2008_04 |
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