関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4,5-Dichloro-3-hydroxypyridazine | HCID 73247 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Benzyl-4,5-dichloro-2,3-dihydropyridazin-3-one | HCID 722438 | 88% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481537B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-9b94d4afb4674eb596256d10c129bba0 |
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| 出典メモ | uspto-grants-2013_07 |
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