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Sodium Acetate → 2-[[3-Methyl-1-(4-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-(2-Oxo-propyl)-benzo[D][1,3]oxazin-4-one | HCID 15938097 | — |
| 反応物 | 4-Hydrazinylpyridine hydrochloride | HCID 22320258 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-[[3-Methyl-1-(4-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid | HCID 22320227 | 49.1% |
反応手順
A solution of 2-(2-oxopropyl)-4H-3,1-benzoxazin-4-one (16.7 g, 82.4 mmol), 4-hydrazinopyridine hydrochloride (12.0 g, 82.4 mmol) and sodium acetate (8.10 g, 98.9 mmol) in ethanol (300 mL) was heated under reflux for 30 minutes. The solution was cooled to room temperature and concentrated under reduced pressure. The residue was poured into water and the resulting crude crystals were collected by filtration. The crystals were washed with ethanol and air dried to give the title compound (11.9 g, 49% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06949648B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-59f508b342ef4dfb8bbe3d56c92b80dc |
| 出典メモ | uspto-grants-2005_09 |