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Potassium Phosphate, Tribasic → (3-(5-Methylpyridin-2-yl)phenyl)methanol
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-Bromo-5-methylpyridine | HCID 564216 | — |
| 反応物 | [3-(Hydroxymethyl)phenyl]boronic acid | HCID 2734662 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (3-(5-Methylpyridin-2-yl)phenyl)methanol | HCID 56604357 | — |
反応手順
92 mg (0.08 mmol) of tetrakis(triphenylphosphine)palladium are added to a suspension, kept under nitrogen, of 849 mg (4.0 mmol) of tripotassium phosphate, 344 mg (2.0 mmol) of 2-bromo-5-methylpyridine and 304 mg (2.0 mmol) of 3-hydroxymethylbenzeneboronic acid in 12 ml of dioxane and 1 ml of water, and the mixture is heated at the boil with stirring for 18 hours. The reaction mixture is cooled to room temperature and partitioned between water and ethyl acetate. The organic phase is dried over sodium sulfate, evaporated, and the residue is chromatographed on a silica-gel column with dichloromethane/methanol as eluent: [3-(5-methylpyridin-2-yl)phenyl]methanol as yellowish oil; LCMS 200.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08435986B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-358414a1b6004d7abe093fc8b5d47d65 |
| 出典メモ | uspto-grants-2013_05 |