関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-Thiocarbonyldi-2(1H)-pyridone | HCID 853162 | — |
| 反応物 | 6-fluoro-1H-indazol-3-amine | HCID 21939267 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178505448 | HCID 178505448 | 73% |
反応手順
To 6-fluoro-1H-indazol-3-amine (0.32 g, 2.1 mmol) in dichloromethane (15 mL) was added 1,1′-thiocarbonyldipyridin-2(1H)-one (0.53 g, 2.30 mmol). The reaction was stirred at 50° C. for 3 hours. The reaction was cooled to room temperature and the crude product was purified by column chromatography (25% ethyl acetate/hexanes) to afford 6-fluoro-3-isothiocyanato-1H-indazole (0.30 g, 1.53 mmol, 73.0% yield) as a light yellow powder. 1H NMR (500 MHz, DMSO-D6) δ ppm 13.39 (s, 1H), 7.78 (dd, J=8.85, 4.88 Hz, 1H), 7.41 (dd, J=9.31, 1.68 Hz, 1H), 7.14 (td, J=9.16, 1.83 Hz, 1H). MS (LC/MS) R.T.=3.69; [M+H]+=194.07.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08309577B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-f8cc5d5354a7474095e94719f3f06d9a |
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| 出典メモ | uspto-grants-2012_11 |
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