関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | (4-Fluorophenyl)hydrazine | HCID 69982 | — |
| 反応物 | 4-Chloro-2-fluoro-5-methoxybenzaldehyde | HCID 14928268 | — |
| 溶媒 | 1-Methylpyrrolidine | HCID 8454 | — |
| 生成物 | 1-(4-Fluorophenyl)-6-chloro-5-methoxy-1H-indazole | HCID 59339887 | — |
反応手順
4-Chloro-2-fluoro-5-methoxy benzaldehyde (204 mg, 1.1 mmol) and 4-fluorophenylhydrazine (176 mg, 1.1 mmol) were dissolved in N-methylpyrrolidine (5 mL). After addition of cesium carbonate (1.15 g, 3.3 mmol) the mixture was heated in a microwave reactor (CEM Discovery, 150 Watt) to 150° C. for 20 min. After dilution with DCM the mixture was washed with sat. NaHCO3, brine and the organic phase was evaporated. After purification of the crude by flash chromatography on silica gel 253 mg (84%) of the subtitle compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728030B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-c1adadd15d2a4e29a6a6d4c16ded8b2c |
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| 出典メモ | uspto-grants-2010_06 |
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