関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | Methyl ((3S,4S)-1-benzyl-4-methylpiperidin-3-yl)carbamate | HCID 56832346 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-benzyl-N,4-dimethylpiperidin-3-amine | HCID 9943889 | 90% |
反応手順
The reduction of cis-(1-benzyl-4-methyl-piperidin-3-yl)-carbamic acid methyl ester was performed by charging 2 grams substrate (1 equiv., 7.62 mmol) to a solution of 20 ml THF (10 volumes) and 15.2 ml 1 M LAH in THF (2 equiv., 15.2 mmol). The addition was performed at a rate so that the temperature reached 30°-40° C. and then the reaction was allowed to cool to 20° C. The reaction was worked up by quenching with 40 ml Rochelle Salt (20 volumes) to a temperature of 35° C. and then extracting the product 2 times into 20 ml methylene chloride (10 volumes). The filtrate was then concentrated to a clear and colorless oil. (90% yield). Note that the starting material needs to be clean in order for this reaction to proceed in high yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084277B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-d62a9641240d4a0b86f430ec8ac9107d |
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| 出典メモ | uspto-grants-2006_08 |
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