関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Barium hydroxide, octahydrate | HCID 17749109 | — |
| 反応物 | 7-Bromo-2-ethyl-4-methoxy-3-nitropyrazolo[1,5-a]pyridine | HCID 21984534 | — |
| 反応物 | 4,6-Dimethyl-2-methoxyphenylboric acid | HCID 21984759 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethylene glycol diethyl ether | HCID 12375 | — |
| 生成物 | 2-Ethyl-4-methoxy-7-(2-methoxy-4,6-dimethylphenyl)-3-nitropyrazolo[1,5-a]pyridine | HCID 21984743 | 98.3% |
反応手順
After adding 4,6-dimethyl-2-methoxyphenylboric acid (191 mg), barium hydroxide octahydrate (334 mg) and tetrakis(triphenylphosphine)palladium (0) complex (123 mg) to a solution of 7-bromo-2-ethyl-4-methoxy-3-nitropyrazolo[1,5-a]pyridine (159 mg) in a mixture of ethyleneglycol diethyl ether (15 mL) and water (7.5 mL), the mixture was heated at 80° C. for 30 minutes. Water was added, extraction was performed with ethyl acetate, the extract was washed with saturated aqueous sodium hydrogencarbonate and brine and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (20 g), and the title compound (185 mg) was obtained from the n-hexane:ethyl acetate (5:1) fraction as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091215B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-b861c7d6b3d849a4a898b1f520c04f67 |
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| 出典メモ | uspto-grants-2006_08 |
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