関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 1-Benzylpiperidine-4-acetonitrile | HCID 562499 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178510845 | HCID 178510845 | — |
反応手順
Sodium metal (0.8 g, 34.78 mmol) was dissolved in dry methanol (10 mL) at 0-10° C. and this solution was added slowly into a suspension of hydroxylamine hydrochloride (2.43 g, 34.96 mmol) in methanol (10 mL) at room temperature. The reaction mixture was stirred for 10 min until a clear solution was obtained, 2-(1-Benzylpiperidin-4-yl)acetonitrile (compound of Example 27; 3 g, 13.99 mmol) in dry methanol (20 mL) was added into the resulting reaction mixture and heated at 75° C. for 13 h. The solvent was evaporated at 50° C. to 55° C. and the crude product obtained was purified by column chromatography (silica gel, chloroform-methanol) to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08629277B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-798425f4702045289f068de3a3155a8c |
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| 出典メモ | uspto-grants-2014_01 |
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