참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formic Acid | HCID 284 | — |
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane | HCID 11626160 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-1-methyl-4-phenylazepane | HCID 21973126 | 67% |
반응 단계
The mixture of Isomer A of 4-((3,5-bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane (3 mg), paraformaldehyde (3 mg) and formic acid (2.2 mg) in chloroform (0.1 mL) was stirred at 65° C. for overnight. After cooling down, the mixture was concentrated under vacuum and filtered through anion exchange cartridge to get rid of formic acid. The crude product was purified by prep TLC with 10% methanol/89% dichloromethane/1% NH4OH to give the product as a clear sticky oil (2 mg, 67% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07098203B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-7c45a7a9c1bb48d9913c24128571cdaf |
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| 출처 메모 | uspto-grants-2006_08 |
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