2-Methylimidazole → 4-chloro-2-methyl-5-(2-methyl-imidazol-1-yl)-2H-pyridazin-3-one
反応式
[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1Cl.[CH3:11][C:12]1[NH:13][CH:14]=[CH:15][N:16]=1>O1CCOCC1>[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[N:13]1[CH:14]=[CH:15][N:16]=[C:12]1[CH3:11]参加物
4
実験手順
A solution of 10.0 g (54.2 mmol) of 4,5-Dichloro-2-methyl-2H-pyridazin-3-one (CAS: [933-76-6]) and 8.90 g (108.4 mmol) of 2-methylimidazole in 50 ml of dioxane was stirred for 16 h at 100° C. The solution was concentrated in vaccuo and the residue was purified by flash chromatography over silicagel using a 95:5 mixture of methylene chloride and methanol as eluant to yield 3.33 g (14.82 mmol, 27%) of the title compound as a white crystalline solid, MS: m/e=225.1, 227.1 (M+H+).
後処理
- concentrationThe solution was concentrated in vaccuo
- customthe residue was purified by flash chromatography over silicagel
- additiona 95:5 mixture of methylene chloride and methanol as eluant
出典と根拠
- ORDレコード
- ord-3d5073b0700e45c4bb21f79808064ccb
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08334287B2
反応ノート
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