HCID 22024596、化合物 → HCID 22024494、化合物
反応式
[Cl:1][C:2]1[C:3]2[N:4]([C:8]([CH:13]([OH:17])[CH2:14][CH2:15][CH3:16])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[CH:6][N:7]=1>C(OCC)(=O)C.C(Cl)Cl.[O-2].[Mn+4].[O-2]>[Cl:1][C:2]1[C:3]2[N:4]([C:8]([C:13](=[O:17])[CH2:14][CH2:15][CH3:16])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[CH:6][N:7]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
The resulting 1-(8-chloro-2-ethylimidazo[1,2-a]pyrazin-3-yl)-1-butanol was dissolved in ethyl acetate (4 mL) and methylene chloride (1 mL), then activated manganese (IV) oxide (3 g) was added thereto, and the mixture was heated under stirring at 60° C. for 5 hours. After being allowed to cool, the reaction mixture was filtered and washed with ethyl acetate, and then the filtrates were combined and evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3) to give the title compound (226 mg) as white crystals.
後処理
- temperaturethe mixture was heated
- temperatureto cool
- filtrationthe reaction mixture was filtered
- washwashed with ethyl acetate
- customevaporated
- customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:3)
出典と根拠
- ORDレコード
- ord-72159f0f66b74005a17e9d77b719b034
- 出典データセット
- uspto-grants-2006_07
- 特許番号
- US07078405B2
反応ノート
読み込み中…