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Dimethylformamide → 5-Fluoro-2-[(1-methyl-1H-pyrazol-5-yl)methoxy]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,5-Difluoropyridine | HCID 2762871 | — |
| 反応物 | (1-methyl-1H-pyrazol-5-yl)methanol | HCID 11815316 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Fluoro-2-[(1-methyl-1H-pyrazol-5-yl)methoxy]pyridine | HCID 86684889 | 58.4% |
反応手順
60% Sodium hydride (390 mg) was added to a dimethylformamide (9.0 mL) solution of (1-methyl-1H-pyrazol-5-yl)methanol (1.00 g) at a room temperature, and the obtained solution was then stirred for 2 hours. Thereafter, 2,5-difluoropyridine (1.17 g) was added to the reaction solution, and the mixed solution was then stirred for 16 hours. Subsequently, water was added to the reaction solution, and the obtained mixture was then extracted with hexane/ethyl acetate (1/2). The organic layer was concentrated under a reduced pressure. The residue was purified by column chromatography (silica gel cartridge, hexane/ethyl acetate=95:5 to 60:40), so as to obtain the title compound (1.08 g) in the form of a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642626B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-c45fde6b78664f38bfbe9e95d356dfa5 |
| 出典メモ | uspto-grants-2014_02 |