反应详情

温度

120 °C

5.0 g of Intermediate B, 2.5 eq of acetophenone, 0.05 eq of Pd2(dba)3, 0.1 eq of BINAP and 2.0 eq of Cs2CO3 were suspended in a mixture of 50 mL toluene and 10 mL of water, then heated to 120° C. under N2 for 60 hours. After cooling to rt, added 100 mL of water and washed the organic phase, dried with anhydrous Na2SO4, concentrated and purified by silica gel column (PE:EA=3:1) to give the pure Intermediate B-1 (1.2 g, 19%) as yellow solid.

1. temperatureAfter cooling to rt
2. washwashed the organic phase
3. dry with materialdried with anhydrous Na2SO4
4. concentrationconcentrated
5. custompurified by silica gel column (PE:EA=3:1)
6. customto give the pure Intermediate B-1 (1.2 g, 19%) as yellow solid