참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzyl Bromide | HCID 7498 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4,5-Dichloro-3-hydroxypyridazine | HCID 73247 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Benzyl-4,5-dichloro-2,3-dihydropyridazin-3-one | HCID 722438 | 88% |
반응 단계
To a mixture of 4,5-dichloro-2H-pyridazin-3-one (3.3 g, 20.0 mmol) and Cs2CO3 (9.77 mg, 1.5 eq) were added DMF (15 mL) and benzyl bromide (3.10 mL, 1.3 eq), which was then stirred for 3 h at 60° C. under nitrogen atmosphere. The mixture was concentrated under reduced pressure, and the residue was extracted twice with ethyl acetate (200 mL). The extract was washed with saturated aqueous sodium hydrogen carbonate solution (NaHCO3, 100 mL×2) and aqueous sodium chloride solution, dried (anhydrous Na2SO4), and concentrated under reduced pressure. The residue was separated by column chromatography (10% ethyl acetate-hexane) to give 4.48 g (88%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08481537B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-9b94d4afb4674eb596256d10c129bba0 |
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| 출처 메모 | uspto-grants-2013_07 |
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