関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane | HCID 11626160 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-1-methyl-4-phenylazepane | HCID 21973126 | 67% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07098203B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-7c45a7a9c1bb48d9913c24128571cdaf |
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| 出典メモ | uspto-grants-2006_08 |
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