関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3-(2-ethoxypyridin-3-yl)-6-fluoro-3-hydroxy-2-oxo-2,3-dihydro-1H-indole-5-carbonitrile | HCID 67087458 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 67087558 | HCID 67087558 | 82.1% |
反応手順
0.47 ml (5.81 mmol) of pyridine was added to 1.3 g (4.15 mmol) of 3-(2-ethoxypyridin-3-yl)-6-fluoro-3-hydroxy-2-oxo-2,3-dihydro-1H-indole-5-carbonitrile in 30 ml of dichloromethane. After the reaction mixture had been cooled to 0° C., 0.42 ml (5.81 mmol) of thionyl chloride was added dropwise. The mixture was stirred at room temperature for one hour and then poured into ice-water. After stirring for 15 minutes, the organic phase was separated off. The aqueous phase was extracted several times with dichloromethane. The combined organic phase was dried over magnesium sulfate and filtered, and the solvent was removed in vacuo. 1.13 g of 3-chloro-3-(2-ethoxypyridin-3-yl)-6-fluoro-2-oxo-2,3-dihydro-1H-indole-5-carbonitrile were obtained as a solid which was employed without further purification in the next stage.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08546401B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-d9000da84ac74eef8bbb16a9175e54bf |
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| 出典メモ | uspto-grants-2013_10 |
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