関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (2E)-3-(dimethylamino)-1-[2-(4-methoxyphenyl)pyrazolo[1,5-b]pyridazin-3-yl]prop-2-en-1-one | HCID 11301707 | — |
| 反応物 | HCID 178418786 | HCID 178418786 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[2-(4-methoxyphenyl)pyrazolo[1,5-b]pyridazin-3-yl]-N-phenylpyrimidin-2-amine | HCID 6539410 | 30% |
反応手順
To a solution of 100 mg (0.31 mmol) of (2E)-3-(dimethylamino)-1-[2-(4-methoxyphenyl)pyrazolo[1,5-b]pyridazin-3-yl]prop-2-en-1-one in 5 ml of N,N-dimethylformamide were added 103 mg (0.39 mmol) of N-phenylguanidinium nitrate and 153 mg (1.11 mmol) of potassium carbonate. The mixture was stirred at 120° C. for 28 hours. Removal of solvent followed by column chromatography with dichloromethane:methanol=100:1 gave the crude product. The crude product was washed with dichloromethane to afford the desired compound in 30% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07582630B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-4401cfab0a2844dca9a7665f338c2c5c |
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| 出典メモ | uspto-grants-2009_09 |
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