3-Oxocyclobutane-1-carbonitrile → 3-(2-(5-Bromo-2-methoxypyridin-3-yl)-2-oxoethylidene)cyclobutanecarbonitrile
反応式
[Br:1][C:2]1[CH:3]=[C:4](/[C:10](/[O-:18])=[CH:11]/P(OC)(OC)=O)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[Li+].O=[C:21]1[CH2:24][CH:23]([C:25]#[N:26])[CH2:22]1>O1CCOCC1.O>[Br:1][C:2]1[CH:3]=[C:4]([C:10](=[O:18])[CH:11]=[C:21]2[CH2:24][CH:23]([C:25]#[N:26])[CH2:22]2)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1参加物
5
反応条件
- 温度
- 120 °C
実験手順
A mixture of lithium (Z)-1-(5-bromo-2-methoxypyridin-3-yl)-2-(dimethoxyphosphoryl)ethenolate (2.0 g, 5.8 mmol) and 3-oxocyclobutanecarbonitrile (1.1 g, 12 mmol) in p-dioxane (6 ml) was heated at 120° C. by Microwave in 1 h. The mixture was cooled, taken up in H2O, extracted with EtOAc (3×), dried over MgSO4, concentrated to provide the title compound. MS (m+1): 307.0.
後処理
- temperatureThe mixture was cooled
- extractionextracted with EtOAc (3×)
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-e212a1b55bb84e838bc9bc9c1b049869
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07951838B2
反応ノート
読み込み中…