Phosphorus oxybromide → 2,6-Dibromopyrido[3,2-d]pyrimidine
反応式
P(Br)(Br)([Br:3])=O.[Br:6][C:7]1[N:8]=[CH:9][C:10]2[N:16]=[C:15](O)[CH:14]=[CH:13][C:11]=2[N:12]=1>CN(C)C=O>[Br:6][C:7]1[N:8]=[CH:9][C:10]2[N:16]=[C:15]([Br:3])[CH:14]=[CH:13][C:11]=2[N:12]=1参加物
4
反応条件
- 温度
- 90 °C
実験手順
A roundbottom flask was charged with N,N-dimethylformamide (4.2 L). Phosphorus oxybromide (646.9 g, 2.26 mol, 2.30 equiv) was added followed by dropwise addition of 2-bromopyrido-[3,2-d]-pyrimidin-6-ol (170 g, 752.1 mmol). The resulting solution was allowed to react, with stirring, for 1 minute while the temperature was maintained at 90° C. The reaction mixture was then quenched by the addition of 10 L of water/ice. The resulting solution was extracted once with ethyl acetate. The organic layer was washed with aqueous NaHSO4 and brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting residue was purified via silica gel chromatography eluting with dichloromethane to afford the title compound.