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HRID 404378作成日:2026年10月25日
Potassium Phosphate, Tribasic → Methyl 4-(5-fluoro-2-methoxypyridin-4-yl)-3-(2-methylbut-3-en-2-yl)benzoate
https://huagongshe.com/reaction/404378
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 反応物 | (5-Fluoro-2-methoxypyridin-4-yl)boronic acid | HCID 44754837 | — |
| 反応物 | Methyl 3-(2-methylbut-3-en-2-yl)-4-(trifluoromethyl-sulfonyloxy)benzoate | HCID 58380282 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-(5-fluoro-2-methoxypyridin-4-yl)-3-(2-methylbut-3-en-2-yl)benzoate | HCID 57467641 | — |
反応手順
The reaction mixture of T45.3 (0.45 g, 1.3 mmol), 5-fluoro-2-methoxypyridin-4-ylboronic acid (0.55 g, 3.2 mmol), potassium phosphate (0.81 g, 3.8 mmol), S-phos (0.11 g, 0.26 mmol) and palladium acetate (0.03 g, 0.13 mmol) in DMF (1.5 mL) was purged with nitrogen three times. The resulting mixture was heated at 90° C. for 2 hours. The mixture was then purified by CombiFlash® silica gel chromatography, eluent with hexane/EtOAc, 9/1 to give T45.4. MS ESI (pos.) m/e: 330.2 (M+H)+. 1H NMR (400 MHz, CDCl3) δ ppm 8.26 (1H, d, J=1.8 Hz), 7.95 (1H, s), 7.90 (1H, dd, J=7.8, 1.8 Hz), 7.06 (1H, d, J=7.8 Hz), 6.59 (1H, d, J=4.9 Hz), 5.88-6.02 (1H, m), 4.75-4.85 (2H, m), 3.95 (3H, s), 3.94 (3H, s), 1.38 (3H, s), 1.36 (3H, s)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08748462B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-9719b670fbc846709b061411a6e4504f |
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| 出典メモ | uspto-grants-2014_06 |
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