関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2,3-Dihydroxyquinoxaline | HCID 27491 | — |
| 反応物 | Pentafluoroethylphenyliodonium trifluoromethanesulfonate | HCID 11488264 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6-pentafluoroethyl-2(1H), 3(4H)-quinoxalinedione | HCID 12871985 | 6% |
反応手順
A mixture of 0.5 g of 2(1H), 3(4H)-quinoxalinedione, 1.60 g of pentafluoroethylphenyliodonium trifluoromethanesulfonate and 10 ml of dimethylformamide was stirred overnight on an oil bath at 45° C. Ethyl acetate was then added to the reaction mixture and the unreacted 2(1H), 3(4H)-quinoxalinedione was removed by filtration (recovery of the starting material: 0.13 g). Water was added to the filtrate and, after rendering the mixture neutral, the mixture was extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and the solvent was distilled off. A small amount of methylene chloride was added to the residue and the precipitated crystals were collected by filtration to obtain 0.05 g of 6-pentafluoroethyl-2(1H), 3(4H)-quinoxalinedione as colorless crystals. Yield 6% (conversion yield, 8%). Melting Point (after recrystallized from acetonitrile): 317°-320° C. (with decomposition).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04324741 |
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| 出典データセット | uspto-grants-1982_04 |
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| ORD ID | ord-31ab1b098c5046459aab17fe543cf85c |
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| 出典メモ | uspto-grants-1982_04 |
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