反应详情

温度

100 °C

Charge a flask with trifluoromethanesulfonic acid 1-[4-(2-azepan-1-yl-ethoxy)-benzoyl]-6-methoxynaphthalen-2-yl ester (3.9 g, 7.06 mmol), 2,6-difluorophenyl boronic acid (2.23 g, 14.12 mmol), potassium phosphate (9.0 g, 42.20 mmol) and tetrakis(triphenylphosphine)palladium (0) (1.63 g, 1.40 mmol) followed by 125 mL dry DMF. Heat the mixture under nitrogen at 100° C. for 90 minutes. Cool, filter, evaporate the solvent and purify on an SCX cartridge, eluting with 2N ammonia/methanol. Purify further on a silica gel column eluting with 0-10% methanol/methylene chloride. The yield is 2.5 g (70%): 1H-NMR (CDCl3, 400 MHz) δ 7.90 (d, J=8.4 Hz, 1H); 7.66-7.61 (m, 3H); 7.39 (d, J=8.4 Hz, 1H); 7.23-7.22 (m, 1H); 7.18-7.08 (m, 2H); 6.79-6.74 (m, 4H); 4.08-4.05 (t, 2H); 3.95 (s, 3H); 2.96-2.89 (t, 2H); 2.78-2.75 (m, 4H); 1.66-1.59 (m, 8H).

1. temperatureCool
2. filtrationfilter
3. customevaporate the solvent
4. custompurify on an SCX cartridge
5. washeluting with 2N ammonia/methanol
6. customPurify further on a silica gel column
7. washeluting with 0-10% methanol/methylene chloride