関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | 1,3-Dibromo-5,5-dimethylhydantoin | HCID 6479 | — |
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-ethyl-7-fluoroquinoxalin-2(1H)-one | HCID 67289205 | — |
| 生成物 | 3-(1-bromoethyl)-7-fluoroquinoxalin-2(1H)-one | HCID 86698519 | 133% |
反応手順
3-Ethyl-7-fluoroquinoxalin-2(1H)-one (20.61 g, 107.2 mmol) and 1,3-dibromo-5,5-dimethylhydantoin (18.77 g, 64.34 mmol) suspended in carbon tetrachloride (1072 ml, 107.2 mmol). To the heterogeneous mixture was added benzoyl peroxide (3.463 g, 10.72 mmol) and the mixture was heated at reflux with stirring (oil bath temperature: 80° C.) for 20 h. After 20 h, the mixture was cooled to rt. After cooling, the mixture was poured into saturated aqueous sodium bicarbonate solution (1 L) with stirring. The precipitate was collected by filtration and washed with water (1 L) to give 3-(1-bromoethyl)-7-fluoroquinoxalin-2(1H)-one (23.19 g, 79.8% yield) as a tan solid:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835432B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-92849659d0874c5281220a124d720487 |
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| 出典メモ | uspto-grants-2014_09 |
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