참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Chloro-4-(chloromethyl)benzene | HCID 7723 | — |
| 반응물 | Azepan-3-amine | HCID 2756445 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Amino-1-(4-chlorobenzyl)homopiperidine | HCID 18426239 | 93% |
반응 단계
A solution of 3-aminohomopiperidine (1.71 g, 15 mmol) in CH3CN (45 mL) was treated with p-chlorobenzyl chloride (463 mg, 2.9 mmol) and K2CO (828 g, 6 mmol) and heated to 70° C. for 9 h. The reaction mixture was cooled to 25° C. and concentrated to afford a yellow solid. The residue was partitioned between H2O (5 mL) and EtOAc (50 mL), and extracted with EtOAc (2×50 mL). The combined organic extracts were washed with brine (20 mL), dried (Na2SO4) and concentrated. The resulting yellow oil was purified by chromatography (SiO2, 5-20% CH3OH—CH2Cl2 gradient elution) to afford the desired product as a yellow oil (639 mg, 93%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06451842B1 |
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| 출처 데이터셋 | uspto-grants-2002_09 |
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| ORD ID | ord-de480b54a84e458c844d9634851ceb4f |
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| 출처 메모 | uspto-grants-2002_09 |
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