反应详情

温度

50 °C

A suspension of title compound 85 (1.75 g, 7.15 mmol) in a solution of sodium formate (2.43 g, 35.8 mmol) in water (32 mL) was stirred at 50° C. for 8 hours and then at room temperature. The reaction mixture was filtered and the resulting solid was dissolved in THF (20 mL), diluted with ethyl acetate (200 mL) then filtered through Celite® and concentrated. The crude residue was triturated in 30% ethyl acetate in hexanes to afford title compound 86 (1.17 g, 78%) as a yellow solid. LRMS (ESI): (calc) 210.08 (found) 211.2 (MH)+. 1H NMR (400 MHz, DMSO-d6) δ (ppm): 9.84 (s, 1H), 7.84 (s, 1H), 7.67 (dd, J=7.9, 1.7 Hz, 1H), 7.33 (ddd, J=8.1, 7.2, 1.8 Hz, 1H), 7.00-6.86 (m, 6H).

1. customat room temperature
2. filtrationThe reaction mixture was filtered
3. dissolutionthe resulting solid was dissolved in THF (20 mL)
4. additiondiluted with ethyl acetate (200 mL)
5. filtrationthen filtered through Celite®
6. concentrationconcentrated
7. customThe crude residue was triturated in 30% ethyl acetate in hexanes