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Ethyl benzoylacetate → HCID 178469958、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl benzoylacetate | HCID 7170 | — |
| 反応物 | ethyl 3-amino-1H-pyrazole-4-carboxylate | HCID 81472 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 178469958 | HCID 178469958 | 61% |
反応手順
Commercially available ethyl 5-amino-1H-pyrazole-4-carboxylate (5.0 g, 32 mmol) was taken into glacial acetic acid (3.2 mL) followed by addition of ethyl 3-oxo-3-phenylpropanoate (6.1 mL, 35 mmol) and the mixture was refluxed for 12 h. The mixture was allowed to cool to room temperature and concentrated in vacuo. The crude solid was recrystallized (ethanol) and collected to yield 3.1 g (61%) of crystalline ethyl 7-hydroxy-5-phenylpyrazolo[1,5-a]pyrimidine-3-carboxylate. 1H NMR (400 MHz, d6-DMSO): 11.75 (s, 1H), 8.28 (s, 1H), 7.80 (m, 2H), 7.61 (m, 3H), 6.28 (s, 1H), 4.31 (q, 2H), 1.34 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08372851B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-d0ac4a62de4d465aa9805715d06346f8 |
| 出典メモ | uspto-grants-2013_02 |