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Water → 4-[2-(2-Fluorophenoxy)ethyl]piperazine-1-carboxylic acid tert-butyl ester
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 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 反応物 | 1-(2-Bromoethoxy)-2-fluorobenzene | HCID 2386106 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[2-(2-Fluorophenoxy)ethyl]piperazine-1-carboxylic acid tert-butyl ester | HCID 67298803 | — |
反応手順
To a solution of piperazine-1-carboxylic acid tert-butyl ester (2.79 g, 15 mmol) and 1-(2-bromoethoxy)-2-fluoro-benzene (3.28 g, 15 mmol) in DMF (6 mL) was added cesium carbonate (Cs2CO3, 9.75 g, 30 mmol). The mixture was stirred at room temperature for a day and then treated with water. The aqueous solution was extracted with ethyl acetate and the extract was washed with water and brine. The organic layer was concentrated and the residue was dried under the vacuum to yield the title compound quantitatively as an oil (5.1 g). 1H NMR (400 MHz, DMSO-d6): δ 1.39 (s, 9H), 2.44 (t, 4H), 2.73 (t, 2H), 3.29 (t, 4H), 4.45 (t, 2H), 6.93 (m, 1H), 7.11 (t, 1H), 7.18 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08183374B2 |
| 出典データセット | uspto-grants-2012_05 |
| ORD ID | ord-7d878bb266584c8b8fb8c18cda8af50d |
| 出典メモ | uspto-grants-2012_05 |