反应详情

Tetrahydrofuran (41 ml), acetonitrile (41 ml) and pyridine (2.07 g) was added to 1-[4-(2-aminopyridin-4-yloxy)-2-fluorophenylcarbamoyl]cyclopropanecarboxylic acid benzyl ester (6.0 g, content 5.51 g), which was dissolved by stirring. Phenyl chloroformate (4.1 g) was added dropwise to this solution with cooling on ice at the internal temperature between 8.8° C. and 14.9° C. The reaction mixture was stirred at the same temperature for 2 hours and 9 minutes, then at room temperature for 3 hours and 5 minutes. The precipitate was collected by filtration, washed with a mixed solvent of tetrahydrofuran and acetonitrile (2:1, 16 ml), and dried under aeration to give the target title compound (6.39 g).

1. dissolutionwas dissolved
2. temperaturewith cooling on ice at the internal temperature between 8.8° C. and 14.9° C
3. stirringThe reaction mixture was stirred at the same temperature for 2 hours and 9 minutes
4. custom5 minutes
5. filtrationThe precipitate was collected by filtration
6. washwashed with a mixed solvent of tetrahydrofuran and acetonitrile (2:1, 16 ml)
7. customdried under aeration