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Sodium hydride → 2-Bromo-6-{[(1,3-dimethyl-1H-pyrazol-5-yl)methoxy]methyl}pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (6-Bromopyridin-2-yl)methanol | HCID 3517811 | — |
| 反応物 | 5-(chloromethyl)-1,3-dimethyl-1H-pyrazole | HCID 4961270 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-6-{[(1,3-dimethyl-1H-pyrazol-5-yl)methoxy]methyl}pyridine | HCID 59526400 | — |
反応手順
To a suspension of NaH (64 mg, 1.59 mmol) in THF (4 mL) at 0° C. under argon was added 5-(chloromethyl)-1,3-dimethyl-1H-pyrazole (230 mg, 1.59 mmol) and allowed to stir for 20 minutes. (6-Bromopyridin-2-yl)methanol (150 mg, 0.80 mmol) was then added and the mixture was allowed to warm to room temperature and then heated to 55° C. overnight. The reaction was then cooled to ambient temperature and quenched by the addition of water. The quenched reaction mixture was diluted with water (10 mL) and DCM (10 mL) and shaken. The suspensions were passed through disposable phase separators and the DCM eluent was captured and evaporated to dryness to afford the title compound which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367706B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-1c4f12a47b554e4ca4a1b2448dbb31cb |
| 出典メモ | uspto-grants-2013_02 |