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2-Toluidine hydrochloride → SK&F 96079
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Toluidine hydrochloride | HCID 12484 | — |
| 反応物 | 4-Chloro-3-(2-chloroethyl)-8-methoxy-2-methylquinoline | HCID 3332664 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | SK&F 96079 | HCID 196776 | 22% |
反応手順
2-Methyl-3-(2-chloroethyl)-4-chloro-8-methoxyquinoline (8.37 g, 31 mmol) and 2-methylaniline hydrochloride (4.45 g, 31 mmol) in 1-butanol (100 ml) were heated at reflux for 5 days, then the solvent evaporated, the crude product taken up in dichloromethane, washed with aqueous sodium bicarbonate, dried and evaporated. Chromatography (silica gel, 2% methanolic ammonia in dichloromethane) and recrystallisation from aqueous ethanol gave 1-(2-methylphenyl)-4-methyl-6-methoxy-2,3-dihydropyrrolo[3,2-c]quinoline (2.04 g, 22 %), m.p. 182°-183°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05051508 |
| 出典データセット | uspto-grants-1991_09 |
| ORD ID | ord-2edeca0174b046659926189dfbd51726 |
| 出典メモ | uspto-grants-1991_09 |