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pentan-3-one O-(2-nitrophenyl)oxime → 2-Ethyl-3-methyl-7-nitrobenzo[b]furan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | pentan-3-one O-(2-nitrophenyl)oxime | HCID 53768417 | — |
| 溶媒 | Hydrochloride methanol | HCID 21893726 | — |
| 生成物 | 2-Ethyl-3-methyl-7-nitrobenzo[b]furan | HCID 70201232 | 91.6% |
反応手順
A mixture of pentan-3-one O-(2-nitrophenyl)oxime (10.50 g) in 10% hydrogen chloride-methanol (105 ml) was refluxed for 4 hours. After concentration in vacuo, the residue was extracted with ethyl acetate and water. The obtained organic layer was washed with saturated aqueous sodium bicarbonate, brine and dried over, sodium sulfate. After evaporation in vacuo, the residue was purified by column chromatography on silica gel (eluate; ethyl acetate:n-hexane=1:6) to give a solid. The resulting solid was triturated with a mixture of ethanol and water (2:1) and the precipitate was collected to give 2-ethyl-3-methyl-7-nitrobenzo[b]furan (4.44 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05858995 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-1ff8c5dfd43a4351aebaadb2017d4f8a |
| 出典メモ | uspto-grants-1999_01 |