関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Chloro-4-(chloromethyl)benzene | HCID 7723 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Piperidinecarboxamide | HCID 92980 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Carbamoyl-1-(4-chlorobenzyl)piperidine | HCID 2845797 | 55.2% |
反応手順
A solution of nipecotamide (6.40 g, 50 mmol) in CH3CN (150 mL) and ethanol (20 mL) was treated with Et3N (7.0 mL, 50 mmol) and 4-chlorobenzyl chloride (8.05 g, 50 mmol). The reaction mixture was stirred at 50° C. for 16 h. After cooling to room temperature, saturated aqueous NaHCO3 (50 mL) and water (150 mL) was added to the reaction mixture. The mixture was extracted with ethyl acetate (150 mL×3) and the combined organic layers were washed with brine, dried (Na2SO4) and concentrated to give a pale red solid. The crude solid was washed with ether (100 mL) to afford 3-carbamoyl-1-(4-chlorobenzyl)piperidine (6.98 g, 54%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06362177B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-6c730d6f69b54ab6a3841806aca31ca0 |
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| 出典メモ | uspto-grants-2002_03 |
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