反应详情

Add a total of 3.4 ml of TFA in several portions at RT to a solution of 1.05 g (2.21 mmol) of tert-butyl rac-3-[(5-bromo-6-phenylfuro[2,3-d]pyrimidin-4-yl)oxy]-1-piperidinecarbamate in 2 ml of dichloromethane, and stir at RT for 2 h. Then dilute with dichloromethane, add satd. sodium hydrogencarbonate solution cautiously to the solution and then wash twice with satd. sodium hydrogencarbonate solution. Dry the organic phase over magnesium sulphate and concentrate under reduced pressure. Stir the oily residue with methanol, filter off the precipitated solid with suction and wash with methanol. Combine mother liquor and wash solution, concentrate under reduced pressure and stir again with a little methanol. Filter off the resulting crystals with suction, wash with methanol and combine with the first crystal fraction. A total of 550 mg (66.4% of theory) of the target compound are obtained.

1. additionadd
2. washsodium hydrogencarbonate solution cautiously to the solution and then wash twice with satd
3. dry with materialDry the organic phase over magnesium sulphate
4. concentrationconcentrate under reduced pressure
5. stirringStir the oily residue with methanol
6. filtrationfilter off the precipitated solid with suction
7. washwash with methanol
8. washCombine mother liquor and wash solution
9. concentrationconcentrate under reduced pressure
10. stirringstir again with a little methanol
11. filtrationFilter off the resulting crystals with suction
12. washwash with methanol
13. customA total of 550 mg (66.4% of theory) of the target compound are obtained