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Hydrochloric Acid → (2,6-Dichloro-5-fluoropyridin-3-yl)methanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,6-Dichloro-5-fluoro-3-pyridinecarbonitrile | HCID 2733849 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (2,6-Dichloro-5-fluoropyridin-3-yl)methanamine | HCID 55255125 | — |
反応手順
To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 6 M HCl (50 ml) and a solution of 2,6-dichloro-5-fluoronicotinonitrile (Aldrich, 10.0 g, 52.4 mmol) in MeOH (100 ml). The mixture was placed under 50 psi H2 on a shaker type Parr apparatus for 21 h, filtered and concentrated. The crude was dissolved in EtOAc, basified with aqueous NaOH, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo to yield the title compound as crude light yellow oil. Used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524917B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-0f8b145b3d1e4d67813cc531a8167cc1 |
| 出典メモ | uspto-grants-2013_09 |