関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Pyridine-2-carboximidamide hydrochloride | HCID 12403615 | — |
| 反応物 | 2-(2-(4-Chlorophenyl)imidazo[1,2-a]pyridin-3-yl)acetohydrazide | HCID 67029159 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178477970 | HCID 178477970 | — |
反応手順
A mixture of 2-(2-(4-chlorophenyl)imidazo[1,2-a]pyridin-3-yl)acetohydrazide (0.55 mmol, 1.0 eq) in DMF (1-2 ml) and picolinimidamide hydrochloride (1.5 eq) was heated at 120° C. for 3 h. The mixture was cooled to rt, treated with sat. NaHCO3 (5 ml), extracted with CH2Cl2 (10 ml). The organic solution was dried with Na2SO4, evaporated under vacuum. The crude product was purified by HPLC. M/e+ 387 for C21H16ClN6 (M+H)+; 1H-NMR (400 MHz, CD3OD) δ 9.11 (d, J=1.4 Hz, 1H), 8.56 (d, J=3.7 Hz, 1H), 8.36 (d, J=6.2 Hz, 2H), 7.77 (d, J=8.4 Hz, 2H), 7.70 (dt, J=8.4, 2.9 Hz, 2H), 7.36 (m, 2H), 6.99 (m, 2H), 4.64 (s, 2H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08497278B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-7298ab0a1a6f476d8420421f50ffba9f |
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| 出典メモ | uspto-grants-2013_07 |
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