참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Cyanobenzoic acid | HCID 15875 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 1-(4-Chlorobenzyl)-4-[(valylamino)methyl]piperidine | HCID 53782731 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 54167831 | HCID 54167831 | — |
반응 단계
Triethylamine (0.011 mL, 0.077 mmol), m-cyanobenzoic acid (28 mg, 0.071 mmol), EDCI (13 mg, 0.065 mmol) and HOBt (9 mg, 0.065 mmol) were added to a dichloromethane (0.60 mL) solution of 1-(4-chlorobenzyl)-4-[(valylamino)methyl]piperidine (20 mg, 0.059 mmol). The resulting reaction mixture was stirred at 25° C. for 16 hours, and the obtained solution was diluted with dichloromethane (0.75 mL), washed with a 2 M aqueous solution of NaOH (0.75 mL×2) and dried by filtration through a PTFE membrane. The dried solution was concentrated to thereby afford 1-(4-chlorobenzyl)-4-[[N-(3-cyanobenzoyl)valyl]aminomethyl]piperidine (Compd. No. 619) (24.2 mg, 88%). Further purification was not required for the resulting compound. The purity was determined by RPLC/MS (85%). ESI/MS m/e 467 (M++H, C26H31ClN4O2).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07390830B1 |
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| 출처 데이터셋 | uspto-grants-2008_06 |
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| ORD ID | ord-9118149ce9c1418c94ac761cef4a7bdc |
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| 출처 메모 | uspto-grants-2008_06 |
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