関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cyclopropanecarboxaldehyde | HCID 123114 | — |
| 反応物 | 1-benzyl-N-methylpiperidin-4-amine | HCID 4136128 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 22712048 | HCID 22712048 | 95% |
反応手順
18.9 g of 1-benzyl-4-methylaminopiperidine in the form of the oil prepared in a) are taken up in 250 ml of methanol, combined with 8.3 g of cyclopropane carboxaldehyde and 11.3 g of sodium cyanoborohydride. The mixture is stirred for 5 hours at 40-50° C., then for about 16 hours at ambient temperature. It is then acidified with 2 N hydrochloric acid, evaporated to dryness in vacuo and the residue is taken up in water. It is washed with ether, made alkaline with concentrated sodium hydroxide solution and extracted with ether/ethyl acetate. The organic extract is dried over sodium sulphate and freed from solvents in vacuo. 22.7 g of 1-benzyl-4-(cyclopropylmethyl-methyl-amino)-piperidine are obtained as a yellowish oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06747044B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-f8daccd7025a4cf39fdc5c8693be6b22 |
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| 出典メモ | uspto-grants-2004_06 |
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