関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Persulfate | HCID 24412 | — |
| 反応物 | 2,3-Dihydro-2,2-dimethyl-7-nitrobenzofuran | HCID 83416 | — |
| 触媒 | Copper sulfate pentahydrate | HCID 24463 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2,3-Dihydro-2,2-dimethyl-7-nitrobenzofuran-3-one | HCID 22404725 | 93.5% |
反応手順
A mixture of 37.3 g (0.193 mole) of 2,3-dihydro-2,2-dimethyl-7-nitrobenzofuran, 156.6 g (0.58 mole) of potassium persulfate, and 48.2 g (0.193 mole) of copper(II) sulfate pentahydrate in 500 mL of acetonitrile and 500 mL of water was prepared. This mixture was heated at reflux for one hour with vigorous stirring. The reaction mixture was cooled and then extracted three times with methylene chloride. The combined extracts were dried over anhydrous magnesium sulfate, filtered, and the solvent was evaporated from the filtrate under reduced pressure, leaving 37.4 g of 2,3-dihydro-2,2-dimethyl-7-nitrobenzofuran-3-one as a residue. The NMR and IR spectra of the same product from a previous run of this reaction were consistent with the proposed structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05521147 |
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| 出典データセット | uspto-grants-1996_05 |
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| ORD ID | ord-f1825f0b5f7f4e1bb24e9f92e97f9cdd |
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| 出典メモ | uspto-grants-1996_05 |
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