참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Bromo-5-nitrothiazole | HCID 18211 | — |
| 반응물 | 6,7-Dimethoxyquinoline-4(1H)-thione | HCID 22936809 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 6,7-Dimethoxy-4-(5-nitrothiazol-2-ylsulfanyl)quinoline | HCID 22936719 | 49% |
반응 단계
After suspending 6,7-dimethoxy-1H-quinoline-4-thione (2.21 g, 10.0 mmol) in dimethylformamide (30 ml), 2-bromo-5-nitrothiazole (2.30 g, 11.0 mmol) was added at 0° C., and then the mixture was stirred at room temperature for 1 hour. The reaction solution was distributed between ethyl acetate and 1N aqueous sodium hydroxide, the organic layer was washed with water and saturated brine and dried over anhydrous magnesium sulfate, the drying agent was filtered off and the filtrate was distilled off under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (eluent—ethyl acetate:hexane=3:1), and the fraction containing the target substance was concentrated, suspended in ethyl acetate and diluted with hexane, after which the crystals were filtered out, washed with hexane and then blow-dried to obtain the title compound (1.70 g, 4.87 mmol, 49%) as light yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07253286B2 |
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| 출처 데이터셋 | uspto-grants-2007_08 |
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| ORD ID | ord-642dfc3b86e64b20ad29127af4685327 |
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| 출처 메모 | uspto-grants-2007_08 |
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