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2-Hydrazinopyridine → HCID 178515860、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Hydrazinopyridine | HCID 78645 | — |
| 反応物 | Ethyl 3-oxo-4-phenylbutanoate | HCID 225855 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178515860 | HCID 178515860 | 30.8% |
反応手順
Compound 2a (1.03 g, 5.0 mmol) prepared in Step 1 of Example A-1 was charged in a 25 mL round-bottom flask and dissolved in 6 mL of ethanol. A solution of 2-hydrazinopyridine (0.55 g, 5.0 mmol, manufactured by Aldrich) in 5 mL of ethanol at 50° C. was gradually added thereto over 30 minutes, followed by reaction for 1 hour. After completion of the reaction was confirmed by TLC, the reaction solution was concentrated by evaporation, extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated, and then purified by column chromatography [n-Hex/EtOAc=3/1 (v/v)] to afford a compound of 3-benzyl-1-(pyridin-2-yl)-1H-pyrazol-5-ol (3a).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637674B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-8c28fcb7cca348d3bd20de67b4acdc17 |
| 出典メモ | uspto-grants-2014_01 |