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3-Azaspiro(5.5)undecane hydrochloride → 3-(4,5-dihydro-1H-imidazol-2-yl)-3-azaspiro[5,5]undecane hydroiodide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Azaspiro(5.5)undecane hydrochloride | HCID 417412 | — |
| 反応物 | 1H-Imidazole, 4,5-dihydro-2-(methylthio)-, hydriodide (1:1) | HCID 12221228 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(4,5-dihydro-1H-imidazol-2-yl)-3-azaspiro[5,5]undecane hydroiodide | HCID 68619688 | 65% |
反応手順
3-Azaspiro[5,5]undecane (0.38 g, 2 mmol) and 2-methylthio-2-imidazoline hydroiodide (0.44 g, 1.8 mmol) was refluxing in CH3OH overnight, concentrated in vacuo and purified by flash chromatography to give yellow oil (0.26 g, 65% yield). 1H NMR (360 MHz, CDCl3) δ 8.27 (br s, 2H), 3.72 (s, 4H), 3.39 (t, J=5.83 Hz, 4H), 1.50 (t, J=5.94 Hz, 4H), 1.47-1.44 (m, 10H); 13C NMR (90 MHz, CDCl3) δ 159.48, 43.39, 42.73, 36.02, 35.26, 30.83, 26.65, 21.61. 21.49; ESI-MS: Calculated for C13H24IN3 (M−I)+ 222.3, Found: 222.5.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08557836B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-3e292b52922e4f0f8ce663087f604858 |
| 出典メモ | uspto-grants-2013_10 |