関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisobutylaluminum hydride | HCID 14487 | — |
| 反応物 | Methyl 4-(oxazol-2-yl)benzoate | HCID 21985208 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Oxazol-2-yl)-benzyl alcohol | HCID 20725624 | 89% |
反応手順
To a solution of methyl-4-(oxazol-2-yl)-benzoate (0.203 g, 1 mmol) in CH2Cl2 (10 mL) 0° C. was added DIBAL-H (4 mL of a 1.0M solution in dichloromethane, 4 mmol) over 10 minutes. The resultant solution was stirred at 0° C. for 2 hours then quenched with an aqueous saturated solution of sodium potassium tartrate (20 mL) and the biphasic mixture stirred rapidly for 60 minutes. The phases were separated and the aqueous layer extracted with CH2Cl2 (3×10 mL). The combined organic fractions were dried (Na2SO4), filtered, concentrated and purified by chromatography on silica gel (10:1 CH2Cl2/MeOH) to afford the title alcohol (0.156 g, 89%). 1H NMR (CDCl3) δ 3.42 (t, 1H, J=6.0 Hz (OH)), 4.77 (s, 2H, J=6.0 Hz), 7.24 (s, 1H), 7.47 (d, 2H, J=7.8 Hz), 7.71 (s, 1H), 8.05 (d, 2H, J=7.8 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091217B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-85cb7c3d3f1440a8a446dd9990ca3e2b |
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| 出典メモ | uspto-grants-2006_08 |
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