関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 反応物 | 2-[4-[4-Methanesulfonyloxybut-1-ynyl]phenyl]-7-methylimidazo[1,2-a]pyridine | HCID 22015608 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-[4-[4-Piperidinobut-1-ynyl]phenyl]-7-methylimidazo[1,2-a]pyridine | HCID 10132217 | 103.2% |
反応手順
The product of Step C (1.00 g) in acetonitrile (15 mL) was treated with piperidine (0.269 g) and potassium carbonate (1.17 g) and heated at reflux for 18 hours. The reaction mixture was cooled to ambient temperature, washed with water (20 mL), dried over magnesium sulfate, filtered and evaporated to give crude product. Silica gel chromatography (methanol/dichloromethane) afforded the title compound (1.0 g). MS (ESI) m/z 344.1 (M+H+). 1H NMR (DMSO) δ 8.23 (d, J=6.95 Hz, 1 H), 8.15 (s, 1 H), 7.73 (d, J=8.37 Hz, 2 H), 7.25 (d, J=8.34 Hz, 2 H), 7.17 (s, 1 H), 6.58 (dd, J=6.9, 1.45 Hz, 1H), 2.33 (m, 6 H), 2.23 (b, 2 H), 2.18 (s, 3 H). 1.33 (pent, 4 H), 1.21 (pent, 2 H). HRMS: MH+ calcd for C23H26N3, 344.2127; found, 344.2134. Analysis: Calc'd for C23H25N3; C, 80.43; H, 7.34; N, 12.23. Found: C, 80.27; H, 7.15; N, 11.81.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07087757B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-6414fe018863447e9a234c42b7b4c928 |
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| 出典メモ | uspto-grants-2006_08 |
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