関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridazine | HCID 9259 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 2-Phenylpyrazolo[1,5-a]pyridine | HCID 15620342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(1-Ethoxycarbonyl-1,4-dihydropyridazin-4-yl)-2-phenylpyrazolo[1,5-a]pyridine | HCID 11791860 | 53.4% |
反応手順
Ethyl chloroformate (3.38 g) was added dropwise with stirring to a solution of 2-phenylpyrazolo[1,5-a]pyridine (2.54 g) and pYridazine (5.00 g) in methylene chloride (5.0 ml) at 10° C. After being stirred at 10° C. for 1 hour and then at room temperature for 2 hours, the reaction mixture was poured onto ice-water (100 ml) and extracted with ethyl acetate. The combined extracts were washed with saturated sodium chloride aqueous solution (100 ml), dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel (150 g) with a mixture of chloroform and n-hexane (1:1) as an eluant. The fractions containing main-product [compound (A)] were combined and evaporated in vacuo to give 3-(1-ethoxycarbonyl-1,4-dihydropyridazin-4-yl)-2-phenylpyrazolo[1,5-a]pyridine (2.42 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04985444 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-15d3dca0671446f8bf98df65312ce056 |
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| 出典メモ | uspto-grants-1991_01 |
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