反应详情

温度

20 °C

A suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one (3.2 g.), methyl 2-isocyanatoacetate (1.4 g.) and triethylamine (1.2 g.) in acetonitrile (50 cc.) is stirred for 18 hours at a temperature of about 20° C. A further amount of methyl 2-isocyanatoacetate (0.7 g.) is added and stirring is continued for a further 3 hours. The precipitate is filtered off and is dissolved in methylene chloride (35 cc.). Decolourising charcoal (0.5 g.) is added. After filtration, diisopropyl ether (105 cc.) is added to the filtrate. The crystalline precipitate which forms is filtered off, washed with diisopropyl ether (15 cc.) and then dried to give 2-(7-chloro-1,8-naphthyridin-2-yl)-3-methoxycarbonylmethylaminocarbonyloxy-isoindolin-1-one (2.5 g.) melting at 208°-210° C.

1. stirringstirring
2. waitis continued for a further 3 hours
3. filtrationThe precipitate is filtered off
4. dissolutionis dissolved in methylene chloride (35 cc.)
5. additionDecolourising charcoal (0.5 g.) is added
6. filtrationAfter filtration, diisopropyl ether (105 cc.)
7. additionis added to the filtrate
8. filtrationThe crystalline precipitate which forms is filtered off
9. washwashed with diisopropyl ether (15 cc.)
10. customdried