関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triacetoxyperiodinane | HCID 159087 | — |
| 反応物 | [5'-Isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-yl]methanol | HCID 53363647 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5'-Isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-carbaldehyde | HCID 57877988 | — |
反応手順
To a solution of 0.725 g of [5′-isopropyl-2′-methoxy-4-(trifluoromethyl)biphenyl-2-yl]methanol in 10 mL of CH2Cl2 was added 1.14 g of Dess-Martin periodinane. The mixture was stirred at room temperature for 30 min, then filtered and concentrated. The residue was purified by flash chromatography on a Biotage Horizon, 40S column, eluting with 1 CV of 1% EtOAc in hexanes, followed by a linear gradient of EtOAc in hexanes from 1 to 100% over 10 CV to provide the title compound. Mass spectrum (ESI) 323.2 (M+1). 1H NMR (500 MHz, CDCl3): δ 9.81 (s, 1H), 8.28 (s, 1H), 7.88 (dd, J=1.5 Hz, 8 Hz, 1H), 7.54 (d, J=8 Hz, 1H), 7.33 (dd, J=2 Hz, 8 Hz, 1H), 7.16 (d, J=2.5 Hz, 1H), 6.95 (d, J=8.5 Hz, 1H), 3.74 (s, 3H), 2.95 (septet, J=7 Hz, 1H), 1.29 (d, J=7 Hz, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08735435B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-3f2abf777bbb4b7ea853106cd8094a9f |
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| 出典メモ | uspto-grants-2014_05 |
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