反应详情

温度

80 °C

A sealed tube was charged with 334h (300 mg, 0.6 mmol), 188e (254 mg, 0.6 mmol), Na2CO3 (129 mg, 1.2 mmol), PdCl2(dppf) (50 mg, 0.06 mmol) suspended in DMF (20 mL), and H2O (1 mL). The mixture was stirred at 80° C. for 5 hours. After reaction the mixture was partitioned between ethyl acetate and water. The organic phase was washed with water (2×), dried over sodium sulfate and concentrated. The residue was purified by reverse phase Combi-flash eluting with 0.3% NH4HCO3 in 1:5 water/CH3CN to give 334i as a brown solid (300 mg, 70%). MS: (M+H)+ 708.

1. customAfter reaction the mixture
2. customwas partitioned between ethyl acetate and water
3. washThe organic phase was washed with water (2×)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe residue was purified by reverse phase Combi-flash
7. washeluting with 0.3% NH4HCO3 in 1:5 water/CH3CN