反应详情

2-Ethyl-4-hydroxythieno[3,2-d]pyrimidine (0.6725 g, 0.00373M) was refluxed with phosphorus oxychloride (20 ml) for 2 hours. The reaction mixture was cooled, concentrated under vacuum, the residue dissolved in methylene chloride, poured over ice and water and basified with ammonia. The layers were separated and the aqueous layer extracted with ether. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated under vacuum to obtain the product, 0.65 g, as a tan solid, m.p. 46°-48° C. the structure of which was confirmed by NMR.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated under vacuum
3. dissolutionthe residue dissolved in methylene chloride
4. additionpoured over ice and water and basified with ammonia
5. customThe layers were separated
6. extractionthe aqueous layer extracted with ether
7. washThe combined organic extracts were washed with brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated under vacuum
10. customto obtain the product, 0.65 g