反应详情

To a mixture of 6-chloro-pyrido[3,2-d]pyrimidin-4(3H)one (3.0 g, 16.5 mmole) and N,N-diisopropylethylamine (9 ml, 50 mmole) in toluene (150 ml), was added POCl3 (4.7 ml, 50 mmol). The resulting reaction mixture was refluxed for 1.5 hour. After cooling to room temperature, the solvent was removed under reduced pressure. The residue was dissolved in dichloromethane (200 ml) and washed with cold water till pH=6-7. The organic phase was dried over MgSO4, filtrated and concentrated under reduced pressure to yield crude 4,6-dichloro-pyrido[3,2-d]pyrimidine which was not purified but used as such for further reactions.

1. customThe resulting reaction mixture
2. temperaturewas refluxed for 1.5 hour
3. customthe solvent was removed under reduced pressure
4. dissolutionThe residue was dissolved in dichloromethane (200 ml)
5. washwashed with cold water till pH=6-7
6. dry with materialThe organic phase was dried over MgSO4
7. filtrationfiltrated
8. concentrationconcentrated under reduced pressure