참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chlorosuccinimide | HCID 31398 | — |
| 반응물 | 6-Methoxy-2-(4-methyl-3-nitrophenyl)imidazo[1,2-b]pyridazine | HCID 68089155 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | 3-Chloro-6-methoxy-2-(4-methyl-3-nitrophenyl)imidazo[1,2-b]pyridazine | HCID 68089122 | 98.9% |
반응 단계
To a stirred solution of 6-methoxy-2-(4-methyl-3-nitrophenyl)imidazo[1,2-b]pyridazine (0.250 g, 0.879 mmol) in acetonitrile (20 mL) is added N-chlorosuccinimide (0.879 mmol) and the mixture is heated at 60° C. for 8 hours. The reaction mixture is diluted with water (50 mL), and sat. aqueous NaHCO3 (50 mL). The precipitate that forms is collected by filtration, washed with water (3×25 mL) and dried under vacuum to give the title compound (0.277 g, 98% yield) as a yellow solid: Rf 0.60 (1:1 EtOAc:hexanes); LCMS (m/z)=319.3, 321.2 [M+H]+, tR=3.02 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08871767B2 |
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| 출처 데이터셋 | uspto-grants-2014_10 |
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| ORD ID | ord-4060c1a9e1d94f638fa118f7ad383a98 |
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| 출처 메모 | uspto-grants-2014_10 |
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