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Ethyl 2-cyano-3-ethoxy-2-butenoate → Ethyl 7-amino-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 2-cyano-3-ethoxy-2-butenoate | HCID 46635 | — |
| 反応物 | HCID 178424562 | HCID 178424562 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 7-amino-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-carboxylate | HCID 22249773 | 20.4% |
反応手順
Concentrated dihydrochloric acid (0.1 mL) was added to a solution of 4-mesityl-3-methyl-1H-5-pyrazoleamine (2.5 g, 11.61 mmol) and ethyl 2-cyano-3-ethoxy-2-butenoate (2.13 g, 11.61 mmol) in ethanol (30 mL), followed by heating under reflux for 18 hours. The reaction mixture was evaporated as it was. Then, water was added and a 5N aqueous solution of sodium hydroxide was added under ice-cooling, to neutralize. Further, the mixture was extracted with ethyl acetate, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (15% ethyl acetate/hexane), to give the title compound (835 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06995163B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-136303b2067444509e1f937d0012b62a |
| 出典メモ | uspto-grants-2006_02 |