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Ethyl Acetate → 7-(2,4-Dichlorophenyl)-2-ethyl-3-nitropyrazolo[1,5-a]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Nitronium tetrafluoroborate | HCID 11073463 | — |
| 反応物 | 7-(2,4-Dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridine | HCID 21984635 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 7-(2,4-Dichlorophenyl)-2-ethyl-3-nitropyrazolo[1,5-a]pyridine | HCID 21984666 | 35.6% |
反応手順
After dissolving 7-(2,4-dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridine (280 mg) in acetonitrile (20 mL), nitronium tetrafluoroborate (255 mg) was added 4 times at 30 minute intervals while stirring on ice. The reaction mixture was added to ice water, extraction was performed with ethyl acetate and the extract was washed with water and brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (115 mg) was obtained from the n-hexane:ethyl acetate (20:1) fraction as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091215B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-b0d69462f11d46589ba57d6318c7fae0 |
| 出典メモ | uspto-grants-2006_08 |