関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (4-Methoxyphenyl)boronic acid | HCID 201262 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 2,2-Dimethyl-5-oxo-2,5-dihydrofuran-3-yl trifluoromethanesulfonate | HCID 58926348 | — |
| 触媒 | Benzyl triethylammonium chloride | HCID 66133 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Toluene water | HCID 22272177 | — |
| 生成物 | 4-(4-methoxyphenyl)-5,5-dimethylfuran-2(5H)-one | HCID 58926254 | — |
反応手順
To a 1:1 mixture of toluene/water (20 mL), were added 2,2-dimethyl-5-oxo-2,5-dihydrofuran-3-yl trifluoromethanesulfonate (100 mg, 0.38 mmol), 4-methoxyphenylboronic acid (87 mg, 0.57 mmol), PdCl2(PPh3)2 (27 mg, 0.038 mmol), 2M KF aqueous solution (0.95 mL, 1.9 mmol), benzyltriethylammonium chloride (8.7 mg, 0.038 mmol). The mixture was heated at 50° C. under N2 for 30 minutes, cooled to room temperature and extracted with EtOAc (2×50 mL). The organic layers were combined, washed with saturated NaHCO3 (50 mL) and brine (50 mL), dried over Na2SO4. Purification through silica gel column with 10-30% EtOAc/hexanes led to the product as yellow solid. Yield: 33 mg, 40%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08877923B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-7bf0b10118034bb1bb14191273d87519 |
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| 出典メモ | uspto-grants-2014_11 |
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