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Hydrochloric Acid → 1-(6-Fluoropyridin-3-yl)ethan-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 2-Fluoro-5-formylpyridine | HCID 16414246 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 生成物 | 1-(6-Fluoropyridin-3-yl)ethan-1-ol | HCID 66600166 | 68% |
反応手順
Add methyl magnesium bromide (3 M in ether, 12 mL, 36 mmol) at 0° C. under nitrogen to a solution of 6-fluoro-pyridine-3-carbaldehyde (3 g, 24 mmol) in THF (20 mL). Continue to stir the mixture for overnight at room temperature. Hydrolyze the mixture with 1 N HCl and follow the basification with diluted ammonium hydroxide to ˜pH 9. Abstract the product with chloroform/isopropyl alcohol (3/1). Dry over sodium sulfate. Concentrate the solution in vacuo to yellow oil. Purify by column chromatography (10% methanol in dichloromethane) to give the product as a colorless oil (2.3 g, 68%). MS (ES) m/z 142 [M+1]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08063212B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-9320ac8ebfc5459a8789f9592ea7f261 |
| 出典メモ | uspto-grants-2011_11 |