Phosphorus oxychloride → 5-Bromo-4-chloro-2-{1-[4-(4-methoxy-benzenesulfonyl)-piperazin-1-yl]-ethyl}-pyrimidine
反応式
[Br:1][C:2]1[C:3](=O)[NH:4][C:5]([CH:8]([N:10]2[CH2:15][CH2:14][N:13]([S:16]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH2:12][CH2:11]2)[CH3:9])=[N:6][CH:7]=1.P(Cl)(Cl)([Cl:30])=O>>[Br:1][C:2]1[C:3]([Cl:30])=[N:4][C:5]([CH:8]([N:10]2[CH2:15][CH2:14][N:13]([S:16]([C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH2:12][CH2:11]2)[CH3:9])=[N:6][CH:7]=1参加物
3
反応条件
- 温度
- 90 °C
実験手順
In a flask containing of 5-bromo-2-{1-[4-(4-methoxy-benzenesulfonyl)-piperazin-1-yl]-ethyl}-3H-pyrimidin-4-one (150.0 mg, 0.33 mmol) in phosphorus oxychloride (2 ml) was heated to 90° C. for 2 hours, then the solvent was concentrated under reduced pressure to give the 5-bromo-4-chloro-2-{1-[4-(4-methoxy-benzenesulfonyl)-piperazin-1-yl]-ethyl}-pyrimidine that was used in the next step without any purification. MS m/z calc. 524.2 found (ESI); 526.2 (M+1)+. Retention time 2.91 minutes.