Phosphorus oxychloride → 4-chloro-N-(1-methyl-1H-pyrazol-4-yl)-7H-pyrrolo[2,3-d]pyrimidin-2-amine
反応式
[CH3:1][N:2]1[CH:6]=[C:5]([NH:7][C:8]2[N:9]=[C:10](O)[C:11]3[CH:16]=[CH:15][NH:14][C:12]=3[N:13]=2)[CH:4]=[N:3]1.O=P(Cl)(Cl)[Cl:20]>>[Cl:20][C:10]1[C:11]2[CH:16]=[CH:15][NH:14][C:12]=2[N:13]=[C:8]([NH:7][C:5]2[CH:4]=[N:3][N:2]([CH3:1])[CH:6]=2)[N:9]=1参加物
3
実験手順
A solution of 2-((1-methyl-1H-pyrazol-4-yl)amino)-7H-pyrrolo[2,3-d]pyrimidin-4-ol (5 g, 0.02 mol) in POCl3 (50 mL) was stirred at 120° C. for 4 hrs. After removal of POCl3 by rotary evaporation, water (37 mL) was added. The pH was adjusted to 10 by aq. NaOH (2 mol/L, 30 mL) and then extracted with EtOAc/THF (2:1, three×200 mL). The combined organic layers were concentrated to dryness to afford the title compound (2.8 g, 56% yield) as a brown solid, which was used as is in the next step.
後処理
- customAfter removal of POCl3
- customby rotary evaporation, water (37 mL)
- additionwas added