関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 3-Methylpyridazine | HCID 74208 | — |
| 反応物 | 2-Phenylpyrazolo[1,5-a]pyridine | HCID 15620342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(3-Methylpyridazin-4-yl)-2-phenylpyrazolo[1,5-a]pyridine | HCID 15158108 | 32% |
反応手順
To a mixture of 2-phenylpyrazolo[1,5-a]pyridine (5.00 g), 3-methylpyridazine (2.90 g) and methylene chloride (20 ml), was added a solution of ethyl chloroformate (5.57 g) in methylene chloride for 17 minutes under ice-cooling and stirred for an hour at the same temperature and then for 6 hours and 40 minutes at room temperature. To the reaction mixture was added methylene chloride (20 ml), and washed with a solution of potassium carbonate (10 ml) and a saturated aqueous solution of sodium chloride (10 ml) and dried over magnesium sulfate. The solvent was removed and chromatographed on silica gel (70 g) with a mixture of n-hexane and ethyl acetate (2:1). The fractions containing the object compound were combined and evaporated in vacuo and recrystallized from a mixture of ethyl acetate and n-hexane to give 3-(3-methylpyridazin-4-yl)-2-phenylpyrazolo[1,5-a]pyridine (2.36 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05155114 |
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| 出典データセット | uspto-grants-1992_10 |
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| ORD ID | ord-729fa189f5d6439ca7a86dbb1b294f72 |
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| 出典メモ | uspto-grants-1992_10 |
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