反应详情

2-bromo-4-(6,6-dimethyl-4-oxo-3-trifluoromethyl-4,5,6,7-tetrahydro-indazol-1-yl)-benzonitrile (500 mg, 1 eq), 3-(2-dimethylamino-ethoxy)-4-methoxy-phenylamine (306 mg, 1.2 eq), Pd(OAc)2 (14 mg), DPPF (66 mg), and NaOtBu (214 mg, 2 eq) were mixed in toluene (5 mL) and microwaved at 140° C. for 25 minutes. Then 10 mL of EtOH(4)/H2O(1) were added, followed by NaOH (700 mg, 2 eq) and H2O2 (1 mL). The mixture was microwaved at 100° C. for 15 min, then concentrated to dryness, and purified by flash chromatography, eluting with 20% EtOH in dichloromethane to give the title compound (480 mg, 71% two-step yield). LCMS (m/z): M+H=560.3.

1. custommicrowaved at 140° C. for 25 minutes
2. customThe mixture was microwaved at 100° C. for 15 min
3. concentrationconcentrated to dryness
4. custompurified by flash chromatography
5. washeluting with 20% EtOH in dichloromethane