5-Bromo-2-(3,3-dimethylbut-1-yn-1-yl)pyrimidine → HCID 57804136、化合物
反応式
Br[C:2]1[CH:3]=[N:4][C:5]([C:8]#[C:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[N:6][CH:7]=1.[Cu](C#N)[C:15]#[N:16]>CN1CCCC1>[CH3:11][C:10]([CH3:13])([CH3:12])[C:9]#[C:8][C:5]1[N:4]=[CH:3][C:2]([C:15]#[N:16])=[CH:7][N:6]=1参加物
4
反応条件
- 温度
- 200 °C
実験手順
A mixture of 5-bromo-2-(3,3-dimethylbut-1-ynyl)pyrimidine (2.5 g, 0.010 mol) and copper cyanide (1.4 g, 0.016 mol) in N-methyl pyrrolidine was heated in a sealed tube at 200° C. for 24 hours. The mixture was allowed to cool to room temperature and filtered through Celite® and the filtrate was concentrated under vaccum. The residue was purified by column chromatography on silica gel with an ethyl acetate: hexane (0-50% gradient) to give the product (1.25 g).
後処理
- temperatureto cool to room temperature
- filtrationfiltered through Celite®
- concentrationthe filtrate was concentrated under vaccum
- customThe residue was purified by column chromatography on silica gel with an ethyl acetate
出典と根拠
- ORDレコード
- ord-7f727b782e1643579291df3acda1962d
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07576099B2
反応ノート
読み込み中…