関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Anisoyl chloride | HCID 7477 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-[2-(2,4-Difluorophenyl)phenyl]ethan-1-amine | HCID 22482376 | — |
| 反応物 | N-[1-(2',4'-difluoro-1,1'-biphenyl-2-yl)ethyl]-4-methoxybenzamide | HCID 68815187 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 4-[(3-fluoro-6-methylphenanthridin-5(6H)-yl)carbonyl]phenol | HCID 11580798 | — |
反応手順
N-[1-(2′,4′-difluoro-1,1′-biphenyl-2-yl)ethyl]-4-methoxybenzamide—The title compound was prepared from 4-methoxybenzoyl chloride (731 mg, 4.28 mmol), 1-(-2′,4′-difluoro-biphenyl-2-yl)-ethylamine (1 g, 4.28 mmol), and triethylamine (717 uL, 5.1 mmol) according to the procedure and in the same manner as described in Example 33, step c. The product was isolated from a Biotage® (40 Mi) column for flash column chromatography (5-30% methyl tert-butylether in hexane) resulting in the isolation of a white solid, 1.53 g (97%). mp 134.5-135° C.; 1H NMR (400 MHz, DMSO-d6) δ ppm 1.29 (d, J=5.43 Hz, 3 H) 3.80 (s, 3 H) 4.96 (m, J=5.95 Hz, 1 H) 6.97 (d, J=9.05 Hz, 2 H) 7.18 (m, 2 H) 7.36 (m, 3 H) 7.64 (d, J=4.14 Hz, 2 H) 7.83 (d, J=7.50 Hz, 2 H) 8.66 (s, 1 H); MS (ESI) m/z 368 ([M+H]+); Anal. calcd for C22H19F2NO2: C:71.92 H:5.21 N:3.81 Found: C:72.11 H:5.23 N:3.77
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07585871B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-3f2ccc82aa80439f8eb29f9c9b3dd79a |
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| 出典メモ | uspto-grants-2009_09 |
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