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Hydrochloric Acid → 4-Pyridin-3-yl-2-pyrimidin-2-yl-1,2-dihydro-3H-pyrazol-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Hydrazinylpyrimidine | HCID 346558 | — |
| 反応物 | 3-Hydroxy-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68708088 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Pyridin-3-yl-2-pyrimidin-2-yl-1,2-dihydro-3H-pyrazol-3-one | HCID 59186971 | — |
反応手順
193 mg (1 mmol) of the compound from Example 2A and 116 mg (1.05 mmol) 2-hydrazinopyrimidine are initially introduced into 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 20 h. 40 mg (1 mmol) sodium hydride suspension (60% strength in paraffin oil) are then added in portions, a significant clouding of the reaction solution developing. The mixture is subsequently stirred at RT for 10 min. 1 ml 1 M hydrochloric acid is then added to the dark reaction mixture, a precipitate separating out. The precipitate is filtered off with suction and the residue is washed with water (2×1 ml) and dried in vacuo. 173 mg (72% of th.) of the title compound are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08252817B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-070ffdff072d47598df30111070eeaa4 |
| 出典メモ | uspto-grants-2012_08 |