反应详情

温度

110 °C

Compound 512 (54 mg, 0.14 mmol) was dissolved in acetonitrile (4 mL) in a reaction vial. Compound 506 (61 mg, 0.21 mmol) and K2CO3 (30 mg, 0.21 mmol) were added. The reaction vial was flushed with argon, closed and then stirred at 110° C. for 50 min. in a microwave oven, followed by reflux in a oil bath for 24 h. The reaction mixture was concentrated in vacuo and purified by continuously gradient flash chromatography using EtOAc/petroleum ether (40-60)(v:v=1:7 to 1:3) as the eluent, affording the title compound as a yellow oil. 13C NMR (CDCl3) δ 190.6, 159.1 (dd), 154.7, 154.5 (d), 154.4 (dd), 147.8, 134.7, 132.9, 129.6, 127.9 (d), 124.4 (dd), 124.2 (dd), 120.6 (d), 117.1 (d), 116.0, 115.1 (d), 112.9, 111.6 (dd), 109.9, 104.9 (dd), 73.9, 69.6, 66.6, 26.8, 25.4

1. customThe reaction
2. customvial was flushed with argon
3. customclosed
4. temperatureby reflux in a oil bath for 24 h
5. concentrationThe reaction mixture was concentrated in vacuo
6. custompurified by continuously gradient flash chromatography