反应详情

温度

0 °C

Mix 3-(4-{[2-(4-chloro-phenyl)-4-(2,2-dimethoxy-ethyl)-thiazole-5-carbonyl]-amino}-2-methoxy-phenoxy)-azetidine-1-carboxylic acid tert-butyl ester (208 g, 344 mmol) in EtOH (2.2 L) and treat with concentrated HCl (208 mL). Heat the mixture to reflux for one hour and then cool to 0° C. Collect the solid by filtration and rinse with ice-cold Et2O (4×500 mL). Dry the solid under vacuum at 55° C. for 2 days to give 159 g (97%) of the title compound as an off-white solid. 1H NMR (300 MHz, DMSO-d6) δ: 9.37 (s, 2H), 8.15 (m, 2H), 7.75 (d, 1H, J=7.6), 7.66 (m, 2H), 7.22 (d, 1H, J=7.5), 7.05 (d, 1H, J=7.3), 7.01 (dd, 1H, J=2.5, 8.7), 6.92 (d, 1H, J=8.6), 5.09 (m, 1H), 4.45 (m, 2H), 4.04 (m, 2H), 3.82 (s, 3H).

1. temperatureHeat the mixture
2. temperatureto reflux for one hour
3. customCollect the solid
4. filtrationby filtration
5. washrinse with ice-cold Et2O (4×500 mL)
6. customDry the solid under vacuum at 55° C. for 2 days