Phosphorus oxychloride → HCID 66839224、化合物
反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[CH:10]/[C:11]([NH2:13])=O)[CH:6]=[CH:5][C:4]=1[N:14]1[CH:18]=[C:17]([CH3:19])[N:16]=[CH:15]1.P(Cl)(Cl)(Cl)=O>>[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[CH:10]/[C:11]#[N:13])[CH:6]=[CH:5][C:4]=1[N:14]1[CH:18]=[C:17]([CH3:19])[N:16]=[CH:15]1参加物
3
反応条件
- 温度
- 90 °C
実験手順
A mixture of (E)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]acrylamide (3.54 g) and phosphorus oxychloride (12 ml) was stirred at 90° C. for one hour. The reaction solution was concentrated under reduced pressure and then diluted with ice water, chloroform and aqueous ammonia, and the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was diluted with ether and the precipitated crystals were collected by filtration. The crystals were washed with ether and then air-dried to obtain 2.27 g of the title compound. The property value of the compound is as follows.