反应详情

A mixture of the product of Step A (0.105 g; 0.27 mmol), the product of Step B (0.08 g; 0.03 mmol) and Cs2CO3 (0.09 g; 0.27 mmol) in anhydrous DMF (1 ml) was stirred overnight at room temperature and solvent was removed in vacuo. The residue was diluted to 15 ml EtOAc and washed with H2O, brine, dried over anhydrous MgSO4, filtered and filtrate evaporated to dryness under reduced pressure. The residue was purified by FCC (SiO2, hexane/EtOAc 9:1) to give the tilted compound (0.12 g; 71%), as colourless solid. 1H-NMR (CDCl3) 1.4 (s, 3H); 1.43 (s, 9H); 1.46 (s, 3H); 2.84 (s, 4H); 2.94 (s, 2H); 3.7 (s, 2H); 3.82 (d, 2H, J=11.5 Hz); 4.07 (d, 2H, J=11.5 Hz); 4.88 (broad s, 1H); 5.07 (s, 2H); 6.74 (d, 1H, J=2.4 Hz); 6.78 (dd, 1H, J=2.4, 8.4 Hz); 6.91 (d, 1H, J=8.4 Hz); 7.29-7.35 (m, 3H); 7.43-7.48 (m, 3H); 7.55 (tr, 1H, J=7.7 Hz); 7.73 (d, 1H, J=7.7 Hz).

1. customsolvent was removed in vacuo
2. additionThe residue was diluted to 15 ml EtOAc
3. washwashed with H2O, brine
4. dry with materialdried over anhydrous MgSO4
5. filtrationfiltered
6. customfiltrate evaporated to dryness under reduced pressure
7. customThe residue was purified by FCC (SiO2, hexane/EtOAc 9:1)
8. customto give the tilted compound (0.12 g; 71%)