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Potassium Carbonate → 8-{2-[4-(2-Fluoro-phenyl)-piperazin-1-yl]-ethyl}-8-aza-spiro[4.5]decane-7,9-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 8-Azaspiro(4.5)decane-7,9-dione | HCID 136843 | — |
| 反応物 | 1-(2-Chloroethyl)-4-(2-fluorophenyl)piperazine | HCID 22074917 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-{2-[4-(2-Fluoro-phenyl)-piperazin-1-yl]-ethyl}-8-aza-spiro[4.5]decane-7,9-dione | HCID 9864325 | 40.3% |
反応手順
A mixture of 3,3-tetramethylene glutarimide (6.9 mg) and potassium carbonate (40 mg) in dimethylformamide (0.5 mL) was stirred at room temperature for 30 minutes. 1-(2-Chloroethyl)-4-(2-fluorophenyl)piperazine (10.0 mg) was added and the resulting solution was heated at 120° C. for 3 hours. The solvent was removed and the residue was purified by thin-layer chomatography (silica gel, eluting with hexane/ethyl acetate, 1:1), giving the title compound as a white solid (6.2 mg, 40%). 1H NMR (300 MHz, CDCl13) δ7.07-6.87 (m, 4H), 3.96 (t, 2H, J=6.6 Hz), 3.05 (t, 4H, J=4.8 Hz), 2.67 (t, 4H, J=4.7 Hz), 2.59 (s, 4H), 2.54 (t, 4H, J=6.6 Hz), 1.73-1.68 (m, 4H), 1.55-1.50 (m, 4H). ESI-MS m/z 374 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706716B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-689b1f30332f48c19fcaf0451b5e9fe2 |
| 出典メモ | uspto-grants-2004_03 |