反应详情

Heat a mixture of 5-chloro-2-(3-methylpyridin-2-yl)-[1,8]naphthyridine (51 mg, 0.2 mmol), 2-amino-5-trifluoromethylpyrazine (42.0 mg, 0.25 mmol), xantphos (11.6 mg, 0.02 mmol); Pd2(dba)3 (18.3 mg, 0.02 mmol)and Cs2CO3 (130 mg, 0.4 mmol) in dioxane (2.0 mL) at 100° C. for 20 hours. Cool the mixture, concentrate under vacuum, dilute with EtOAc/water (5.0 mL each), filter through celite, wash celite with EtOAc (2×5 mL) and dry the combined organic layers with MgSO4. Filter the dried extract and concentrate under vacuum to afford the crude product. Purify by preparative TLC using 2% MeOH/EtOAc as eluent to afford the title compound as a yellow solid. 1H NMR (400 MHZ, DMSO-D6) δ 10.6 (s, 1H), 9.04 (d, 1H, J=2.1 Hz), 9.0 (s,1H), 8.77 (s, 2H), 8.59 (d, 1H, J=1.6 Hz), 8.4 (s, 1H), 8.20 (d, 1H, J=2.2 Hz), 7.81(d, 1H, J=1.9 Hz), 7.42 (dd, 1H), 2.65 (s, 3H). MS=383.11 (M+H).

1. temperatureHeat
2. temperatureCool the mixture
3. concentrationconcentrate under vacuum
4. additiondilute with EtOAc/water (5.0 mL each)
5. filtrationfilter through celite
6. washwash celite with EtOAc (2×5 mL)
7. dry with materialdry the combined organic layers with MgSO4
8. filtrationFilter the dried
9. extractionextract
10. concentrationconcentrate under vacuum
11. customto afford the crude product
12. customPurify by preparative TLC