反应详情

Heat a mixture of 550 mg (1.47 mmol) of rac-5-bromo-6-phenyl-4-(piperidin-3-yloxy)furo[2,3-d]-pyrimidine, 532 mg (2.94 mmol) of 4-bromobutyric acid methyl ester, 24.4 mg (0.147 mmol) of potassium iodide and 0.77 ml (4.41 mmol) of N,N-diisopropylethylamine in 1.5 ml of THF under reflux for 2 h. After cooling, dilute with dichloromethane and add to water. After phase separation, extract the aqueous phase with dichloromethane. Combine the organic phases, wash with satd. sodium hydrogencarbonate solution, dry over magnesium sulphate and concentrate under reduced pressure. From the residue, after purification by preparative RP-HPLC (eluent: acetonitrile/water), 780 mg of the target product are isolated, which are used without further purification.

1. temperatureHeat
2. temperatureunder reflux for 2 h
3. temperatureAfter cooling
4. customAfter phase separation
5. extractionextract the aqueous phase with dichloromethane
6. washwash with satd
7. dry with materialsodium hydrogencarbonate solution, dry over magnesium sulphate
8. concentrationconcentrate under reduced pressure
9. customFrom the residue, after purification by preparative RP-HPLC (eluent: acetonitrile/water), 780 mg of the target product
10. customare isolated
11. customwhich are used without further purification