反应详情

To a solution of (R)-5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidine-3-carboxylic acid (Preparation C, 20.0 mg, 0.058 mmol) and HATU (24.3 mg, 0.064 mmol) in dry DMF (0.4 mL) was added tert-butyl amine (12.7 mg, 0.174 mmol) followed by diisopropylethylamine (22.5 mg, 0.174 mmol). The mixture was stirred under an atmosphere of N2 for 18 hours and was added to H2O (3 mL) and mixed. The mixture was extracted with EtOAc and combined extracts were washed with 1M HCl, H2O, saturated NaHCO3 and dried over MgSO4. The solution was eluted through a SPE SiOH column eluting first with 50% EtOAc-hexanes then with EtOAc. The EtOAc pool was concentrated and the residual colorless glass was treated with hexanes give a white suspension. The hexanes were removed, and the solid was washed with hexanes and dried in vacuum to afford the title compound as a white solid (20 mg, 90%). MS (apci) m/z=400.1 (M+H).

1. additionmixed
2. extractionThe mixture was extracted with EtOAc
3. washwere washed with 1M HCl, H2O, saturated NaHCO3
4. dry with materialdried over MgSO4
5. washThe solution was eluted through a SPE SiOH column
6. washeluting first with 50% EtOAc-hexanes
7. concentrationThe EtOAc pool was concentrated
8. additionthe residual colorless glass was treated with hexanes
9. customgive a white suspension
10. customThe hexanes were removed
11. washthe solid was washed with hexanes
12. customdried in vacuum