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1-Butanol → 5-Butoxy-2-nitrobenzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-Fluoro-2-nitrobenzoic acid methyl ester | HCID 5152049 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-Butoxy-2-nitrobenzoic acid methyl ester | HCID 68976499 | — |
反応手順
Sodium hydride (302.4 mg) was added to a solution of 1-butanol (0.634 mL) in DMF (15 mL). The reaction mixture was stirred until there was no further evolution of CO2 and then 5-fluoro-2-nitrobenzoic acid methyl ester (1.15 g) was added and the mixture was stirred at room temperature overnight. The reaction was then mixed with ethyl acetate, washed with 10% sodium bicarbonate and 10% citric acid solution, dried over sodium sulfate and concentrated. The crude product was purified by preparative HPLC. The product with the molecular weight of 253.26 (C12H15NO5) was obtained in this way; MS (ESI): 254 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08828991B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-bb61bd3967b346ddbd2607904150f60b |
| 出典メモ | uspto-grants-2014_09 |