反应详情

温度

87.5 °C

To a four-neck round-bottom 250 ml flask equipped with mechanical stirring and condenser were added at 20-25° C. and under nitrogen atmosphere Xantphos, palladium acetate, tripotassium phosphate trihydrate, PVP, 4-bromophenyl methyl sulfone, 5-acetyl-2-methyl pyridine, water (50.00 ml). A vacuum/nitrogen cycle was repeated for at least three times at 20-25° C. The resulting reaction mixture was heated up to 85-90° C. and stirred for at least 24 h. The reaction mixture was transferred in an other recipient then cooled down to 40-50° C. and diluted with water (400 ml). The resulting mixture was stirred at 40-45° C. for 15 min and cooled down to −5-0° C. The resulting reaction mixture was stirred at −5-0° C. for at least 2 h, then it was filtered and the cake was washed with water (3×100 ml) and dried at 65-70° C. under reduced pressure to afford a crude product of formula (I) as a yellow solid (48.3 g). yield: 90.1%, Purity: 75.7% by HPLC A %.

1. customTo a four-neck round-bottom 250 ml flask equipped
2. customwas repeated for at least three times at 20-25° C
3. customThe resulting reaction mixture
4. stirringstirred for at least 24 h
5. temperaturethen cooled down to 40-50° C.
6. stirringThe resulting mixture was stirred at 40-45° C. for 15 min
7. temperaturecooled down to −5-0° C
8. customThe resulting reaction mixture
9. stirringwas stirred at −5-0° C. for at least 2 h
10. filtrationit was filtered
11. washthe cake was washed with water (3×100 ml)
12. customdried at 65-70° C. under reduced pressure