反应详情

6-Benzyloxy4-hydroxy-pyrido[3,4-d]pyrimidine (1.033 g, 4.1 mmol) was suspended in thionyl chloride (10 ml) under a nitogen atmosphere. DMF (3 drops) was added and the mixture was heated to reflux with stirring for 5.5 hours to give a dark solution, and then left to stand under nitrogen overnight. The mixture was concentrated in vacuo, azeotroping twice with toluene to remove all traces of thionyl cloride and acidic by-products. The material was further dried for two hours in vacuo to give the title compound as a brown solid, used without further purification; δH [2H6]DMSO 8.77(1H,s), 8.13(1H,s), 7.30-7.52 (6H,m), 5.45 (2H,s).

1. temperaturethe mixture was heated
2. temperatureto reflux
3. customto give a dark solution
4. waitleft
5. waitto stand under nitrogen overnight
6. concentrationThe mixture was concentrated in vacuo
7. customazeotroping twice with toluene
8. customto remove all traces of thionyl cloride and acidic by-products
9. customThe material was further dried for two hours in vacuo