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4-Aminothiophenol → 2-(4-Aminophenylthio)-4-ethoxycarbonylquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminothiophenol | HCID 14510 | — |
| 反応物 | Ethyl 2-chloroquinoline-4-carboxylate | HCID 230586 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(4-Aminophenylthio)-4-ethoxycarbonylquinoline | HCID 18971646 | 36% |
反応手順
2-Chloro-4-ethoxycarbonylquinoline (0.024 moles, 5.56 g), 4-aminothiophenol (0.024 moles, 3.0 g) and 4-dimethylaminopyridine (0.024 moles, 2.9 g) were stirred in 250 ml ethanol for 3 days. The reaction mixture was filtered, concentrated, ethyl acetate added, washed with water and dried over sodium sulfate. The solution was concentrated and the product purified by HPLC over silica gel eluted with 25% ethyl acetate/hexane to yield 2-(4-aminophenylthio)-4-ethoxycarbonylquinoline 2.8 g, 36%. Mass Spec (FD) 324. Calculated for C18H16N2O2S: C, 66.64; H, 4.97; N, 8.63. Found: C, 66.50; H, 5.00 N, 8.54.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624937 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-603b04cd056d463f8fd093942204d27e |
| 出典メモ | uspto-grants-1997_04 |