참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 2-Methyl-1,3-cyclohexanedione | HCID 70945 | — |
| 반응물 | Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1) | HCID 71600 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 2-chloro-8,9-dihydro-10-methylpyrido[1,2-a]indol-6(7H)-one | HCID 10353960 | 50% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05290785 |
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| 출처 데이터셋 | uspto-grants-1994_03 |
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| ORD ID | ord-2e52c32915dd405ea0771bfe9e44394c |
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| 출처 메모 | uspto-grants-1994_03 |
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