反应详情

A 3 N HCl solution in 1,4-dioxane (0.4 mL) was slowly added to a solution of tert-butyl 4-(4-((tert-butoxycarbonyl (2-chloro-4-(3-(5-cyanopyrazin-2-yl)ureido)-5-methoxy-phenethyl)amino)methyl)phenyl)piperazine-1-carboxylate (0.1 g) in acetonitrile (5 mL) at 0° C. The mixture was allowed to warm to room temperature and then stirring continued for one hour. Diethyl ether (25 mL) was added and after stirring continued for 15 minutes then the supernatant was decanted and the resulting solid was triturated with diethyl ether (25 mL) and dried under reduced pressure to yield a yellow solid. The solid was further triturated with methanol followed by diethyl ether and dried under reduced pressure to give the title compound (0.05 g, 60%) as an off-white solid.

1. stirringafter stirring
2. waitcontinued for 15 minutes
3. customthe supernatant was decanted
4. customthe resulting solid was triturated with diethyl ether (25 mL)
5. customdried under reduced pressure
6. customto yield a yellow solid
7. customThe solid was further triturated with methanol
8. customdried under reduced pressure