関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-(3-hydroxyphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide | HCID 19481482 | — |
| 反応物 | (6-Iodoimidazo[1,2-b]pyridazin-2-yl)methanol | HCID 57441048 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-{[2-(hydroxymethyl)imidazo[1,2-b]pyridazin-6-yl]oxy}phenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide | HCID 57505461 | 13% |
反応手順
To a solution of (6-iodoimidazo[1,2-b]pyridazin-2-yl)methanol (400 mg, 1.45 mmol) in N,N-dimethylformamide (4.0 mL) were added N-(3-hydroxyphenyl)-1,3-dimethyl-1H-pyrazole-5-carboxamide (504 mg, 2.18 mmol) and potassium carbonate (402 mg, 2.91 mmol), and the mixture was stirred at 150° C. for 16 hr. After cooling the mixture to room temperature, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate/tetrahydrofuran, washed with saturated brine, dried over anhydrous sodium sulfate, and filtrated. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/ethanol=100/0→10/1) to give the title compound (70 mg, 13%) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08044049B2 |
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| 出典データセット | uspto-grants-2011_10 |
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| ORD ID | ord-def0a9d79033427d9da5cbc9359dfa4b |
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| 出典メモ | uspto-grants-2011_10 |
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