関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Bromoethyl methyl ether | HCID 80972 | — |
| 反応物 | HCID 178418997 | HCID 178418997 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Bromo-1-(2-methoxyethyl)-3-nitropyridin-2(1H)-one | HCID 22293279 | 58.4% |
反応手順
Cesium carbonate (14.88 g, 45.66 mmol) was added to a solution of 5-bromo-3-nitropyridin-2-ol (10.0 g, 45.7 mmol) and 2-bromoethyl methyl ether (4.29 mL, 45.66 mmol) in N,N-dimethylformamide (400 mL). After 3 h, additional 2-bromoethyl methyl ether (4.29 mL, 45.7 mmol) was added, and the reaction was heated to 60° C. After 4 h, water was added. The mixture was extracted with ethyl acetate (3×), and the combined organic extracts were washed with saturated brine, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% hexanes→40% ethyl acetate/hexanes) gave the title compound (7.39 g). MS 277 (M).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07772224B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-74e50137ada74bfa8b7a7c5968c80192 |
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| 出典メモ | uspto-grants-2010_08 |
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