反应详情

温度

200 °C

4-Bromo-6-(5-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (250 mg, 0.768 mmol), (R)-1-(6-(trifluoromethyl)pyridin-3-yl)ethanamine (219 mg, 1.15 mmol), N,N-diisopropylethylamine (401 μL, 2.30 mmol), and acetonitrile (0.75 mL) were added to a 0.5-2 mL microwave vial. The reaction was heated in the microwave reactor at 200° C. for 2.5 hours. The solids were filtered from solution and washed with acetonitrile (2×0.5 mL) and ether (2×3 mL) (219 mg of a light yellow solid). The filtrate was evaporated and the residue was redissolved in CH2Cl2 (10 mL) and washed with 1M NaH2PO4 (2×8 mL). The organic layer was dried with Na2SO4, filtered and evaporated to give an orange solid. The crude product was purified by column to give 67 mg of a light yellow solid. The 2 products that were obtained were combined (219 mg+67 mg). To remove some of the yellow colored impurity, ethyl ether (3 mL) was added and the mixture was stirred for about 1 hour then the solution was decanted from the solids. The solids were washed with ethyl ether (2×2 mL) to yield a light beige solid (264 mg, 79% yield).

1. filtrationThe solids were filtered from solution
2. washwashed with acetonitrile (2×0.5 mL) and ether (2×3 mL) (219 mg of a light yellow solid)
3. customThe filtrate was evaporated
4. dissolutionthe residue was redissolved in CH2Cl2 (10 mL)
5. washwashed with 1M NaH2PO4 (2×8 mL)
6. dry with materialThe organic layer was dried with Na2SO4
7. filtrationfiltered
8. customevaporated
9. customto give an orange solid
10. customThe crude product was purified by column