反应详情

温度

100 °C

A mixture of N-(2-iodo-5-methoxyphenyl)acetamide (0.45 g; 1.55 mmol), 3-(tert-butyldimethylsilyl)-1-(3,4,5-trimethoxyphenyl)prop-2-yn-1-one (0.5 g; 1.51 mmol), LiCl (0.069 g; 1.6 mmol) and Na2CO3 (0.477 g; 4.5 mmol) in anhydrous DMF (8 ml) was degassed with N2 and temperature was raised to 100° C. with stirring. Pd(OAc)2 (0.15 g) was added and heating was continued for 1.5 h. The solvent was removed in vacuo and the residue was diluted to 100 ml with EtOAc. This was washed with H2O, dried over MgSO4, filtered and the filtrate was evaporated to dryness. The residue was purified by FCC (SiO2) to give the desired product (0.53 g; 69%) as creamy gum. 1H-NMR (CDCl3) 0.12 (s, 6H); 0.98 (s, 9H); 2.84 (s, 3H); 3.77 (s, 3H); 3.86 (s, 6H); 3.93 (s, 3H); 6.8 (dd, 1H, J=2.07, 8.73 Hz), 7.00 (d, 1H, J=8.73 Hz), 7.16 (broad s, 3H).

1. customwas degassed with N2 and temperature
2. additionPd(OAc)2 (0.15 g) was added
3. temperatureheating
4. customThe solvent was removed in vacuo
5. additionthe residue was diluted to 100 ml with EtOAc
6. washThis was washed with H2O
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. customthe filtrate was evaporated to dryness
10. customThe residue was purified by FCC (SiO2)