反应详情

温度

120 °C

A 5-mL reaction vial equipped with a magnetic stirrer was charged with compound 138 (200 mg, 0.300 mmol), tetrakis(triphenylphosphine)palladium (34.0 mg, 0.029 mmol), zinc cyanide (70 mg, 0.60 mmol) and anhydrous DMF (1 mL). The vial was purged with nitrogen, heated to 120° C. for 3.5 h then cooled to ambient temperature and poured into a saturated aqueous sodium bicarbonate solution (25 mL). The resulting suspension was extracted with methylene chloride (3×20 mL), and the organic extracts were combined, dried over sodium sulfate and filtered. Concentration of the filtrate followed by purification by column chromatography gave a 66% yield of compound 141 as a white solid. 1H NMR (CDCl3) δ (ppm) 8.30 (d, 1H, J=6.9 Hz), 7.58-8.02 (m, 7H), 7.30 (d, 1H, J=7.0 Hz), 5.60 (s, 2H), 5.07 (bs, 1H), 3.65 (m, 2H), 2.84 (s, 3H), 1.58 (d, 38, J=6.7 Hz), 0.96 (m, 2H), 0.02 (s, 9H).

1. customA 5-mL reaction
2. customvial equipped with a magnetic stirrer
3. customThe vial was purged with nitrogen
4. temperaturethen cooled to ambient temperature
5. additionpoured into a saturated aqueous sodium bicarbonate solution (25 mL)
6. extractionThe resulting suspension was extracted with methylene chloride (3×20 mL)
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customConcentration of the filtrate followed by purification by column chromatography