참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Chloro-4-(chloromethyl)benzene | HCID 7723 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Piperidinecarboxamide | HCID 92980 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Carbamoyl-1-(4-chlorobenzyl)piperidine | HCID 2845797 | 55.2% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06362177B1 |
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| 출처 데이터셋 | uspto-grants-2002_03 |
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| ORD ID | ord-6c730d6f69b54ab6a3841806aca31ca0 |
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| 출처 메모 | uspto-grants-2002_03 |
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