関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl 5-fluoro-2-(pyrimidin-2-yl)benzoate | HCID 67086501 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Fluoro-2-(pyrimidin-2-yl)benzoic acid | HCID 67086950 | 83% |
反応手順
To a solution of 5-fluoro-2-pyrimidin-2-yl-benzoic acid methyl ester (1.72 g, 7.407 mmol) in 2-methyl-THF (20 mL) was added sodium hydroxide (0.74 g, 18.517 mmol) and water (20 mL). The mixture was heated to 72° C. and stirred for 2 h. The layers were separated and the aqueous layer was extracted with additional MTBE. A 50% HCl(aq) solution was then dripped into the aqueous layer until a pH of 1 was reached. The resulting solids were filtered to provide the desired product as an off-white solid (1.34 g, 83% yield). 1H NMR (400 MHz, CD3OD): 8.82 (d, J=5.0 Hz, 2H), 7.89 (dd, J=8.6, 5.4 Hz, 1H), 7.53 (dd, J=9.0, 2.7 Hz, 1H), 7.39 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09062044B2 |
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| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-588f43ceacf44d6cafa224c289cdd807 |
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| 出典メモ | uspto-grants-2015_06 |
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