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Lithium hydroxide, monohydrate → 1-(Difluoromethyl)-6-oxo-1,6-dihydropyridine-3-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | HCID 16079629 | HCID 16079629 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(Difluoromethyl)-6-oxo-1,6-dihydropyridine-3-carboxylic acid | HCID 21885875 | — |
反応手順
To a solution of methyl 1-(difluoromethyl)-6-oxo-1,6-dihydropyridine-3-carboxylate (0.500 g, 2.461 mmol) in MeOH (12 mL) and water (4 mL) was added lithium hydroxide hydrate (0.207 g, 4.92 mmol, Aldrich). The resulting mixture was then stirred at room temperature for 4 h. Solvent (MeOH) was removed in vacuok, and the remaining aqueous solution was adjusted to pH=5-6 by addition of concentrated HCl. The mixture was then extracted with EtOAc (3×10 mL). The combined organic layers were dried (MgSO4), and the solvent removed to give the title compound as a yellow solid. MS (ESI, positive ion) m/z: 190 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08710043B2 |
| 出典データセット | uspto-grants-2014_04 |
| ORD ID | ord-11feac23ce4f4d39a84df5b83992595a |
| 出典メモ | uspto-grants-2014_04 |