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Sulfuric Acid → 2-chloro-8,9-dihydro-10-methylpyrido[1,2-a]indol-6(7H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Methyl-1,3-cyclohexanedione | HCID 70945 | — |
| 反応物 | Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1) | HCID 71600 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-chloro-8,9-dihydro-10-methylpyrido[1,2-a]indol-6(7H)-one | HCID 10353960 | 50% |
反応手順
To a suspension of p-chlorophenylhydrazine hydrochloride (8.52 g) in toluene (100 ml) were added 2-methylcyclohexane-1,3-dione (5.0 g) and 40% sulfuric acid (40 ml), and the mixture was stirred at 80°-85° C. for 4 hours. After cooling, the organic layer was separated. The aqueous layer was extracted with toluene. The organic layers were combined and washed with aqueous sodium bicarbonate, water, and brine. After dried over sodium sulfate, the organic layer was evaporated. The residue was recrystallized from methanol to give 2-chloro-8,9-dihydro-10-methylpyrido[1,2-a]indol-6(7H)-one (4.63 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05141945 |
| 出典データセット | uspto-grants-1992_08 |
| ORD ID | ord-068d60d0660840e496a0579eca6f0f35 |
| 出典メモ | uspto-grants-1992_08 |