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Water → 1-[2-(1,3-Dioxolan-2-yl)ethyl]-6-fluoroquinoxalin-2(1H)one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium hydride | HCID 62714 | — |
| 反応物 | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| 反応物 | 6-Fluoro-1,2-dihydroquinoxalin-2-one | HCID 12686386 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[2-(1,3-Dioxolan-2-yl)ethyl]-6-fluoroquinoxalin-2(1H)one | HCID 86725009 | 32% |
反応手順
Lithium hydride (57 mg, 7.3 mmol) was added to a solution of 6-fluoroquinoxalin-2(1H)one (1 g, 6.0 mmol) in N,N-dimethylformamide (6 ml) under cooling on ice and the mixture was stirred at room temperature for 30 minutes. The mixture was cooled on ice again and a solution of 2-(2-bromoethyl)-1,3-dioxolane (0.88 ml, 7.3 mmol) in N,N-dimethylformamide (2 ml) was gradually added thereto and the mixture was stirred for 4 hours. Water was added thereto, the mixture was then extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to yield 0.5 g (32%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08952010B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-6d0acef788034ee3b21b7f58af07c8d3 |
| 出典メモ | uspto-grants-2015_02 |