preparation | the preparation of xikangning is as follows: compound 7(91.0g,0.5mol), HCHO solution (81g,1.0mol),HCl(80g,0.8mol) and AcOH(200g) are heated at 50~60 ℃ for 24 hours, A clear solution was obtained and then poured into cold water (1kg). The obtained solid was collected by suction filtration, washed with water (60g × 3), and dried at 50 ℃ to obtain crude corning 8(95g), which was a brown solid, and was purified (180g) by recrystallization from 90% MeOH/H2O to obtain purified corning 8(71.8g,74%), which was a white solid. Melting point 100~101 c. 1HNMR(300Hz,CDCl3):δ3.92(s,3H),4.11(s,3H),5.20(s,2H),7.09(d,1H,J = 8.2Hz),7.25(d,1H,J = 8.2Hz). ESI-MS(m/z):217.0(M Na),411.0(2M Na). |