Phosphorus oxychloride → HCID 59846662、化合物
反応式
[CH2:1]([C:3]1[NH:8][C:7](=O)[CH:6]=[C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])[N:4]=1)[CH3:2].P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:7]1[CH:6]=[C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])[N:4]=[C:3]([CH2:1][CH3:2])[N:8]=1参加物
3
実験手順
A solution of 2-ethyl-6-(2-methoxy-phenyl)-3H-pyrimidin-4-one (1.1 g, 4.9 mmol) and phosphorous oxychloride (3.0 mL, 32 mmol) was refluxed for four hours. After cooling to ambient temperature the reaction mixture was concentrated in vacuo and the resultant residue was diluted with dichloromethane. The organics were washed with ice-water. After extraction of the aqueous layer with dichloromethane the combined organics were washed with brine and dried over sodium sulfate. Following Si gel chromatography (1:5 ethyl acetate:hexanes) 0.91 g (74%) of the title compound was isolated as a pale yellow oil.
後処理
- concentrationwas concentrated in vacuo
- additionthe resultant residue was diluted with dichloromethane
- washThe organics were washed with ice-water