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Potassium Carbonate → 3-(2-Ethoxyphenyl)-3-hydroxy-2-oxo-1-(quinoline-8-sulfonyl)-2,3-dihydro-1H-indole-5-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 8-Quinolinesulfonyl chloride | HCID 29220 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 5-Cyano-3-(2-ethoxyphenyl)-3-hydroxy-indol-2-one | HCID 66593041 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(2-Ethoxyphenyl)-3-hydroxy-2-oxo-1-(quinoline-8-sulfonyl)-2,3-dihydro-1H-indole-5-carbonitrile | HCID 69070553 | 68.3% |
反応手順
2.3 g (10.6 mMol) of potassium tert-butanolate are added to 5.5 g (18.7 mMol) of the intermediate 1b in 40 ml of DMF at 0° C. The reaction mixture was stirred for 1 h. Then 4.25 g (18.7 mMol) of 8-quinolinesulfonyl chloride were added at 0° C. The reaction solution was stirred at 0° C. for three hours and then at room temperature for 16 h. This reaction solution was poured into aqueous K2CO3 solution, resulting in a precipitate which was isolated. This solid was dissolved in methylene chloride, dried and concentrated in vacuo. The resulting residue was recrystallized from ethanol. 6.2 g of the product were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202870B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-1271c5c5631b453f93aa8785d671661c |
| 出典メモ | uspto-grants-2012_06 |