Pyridine → Benzyl 1-({[4-([2-[(phenoxycarbonyl)amino]pyridin-4-yl}oxy)-2,5-difluorophenyl]amino}carbonyl)cyclopropanecarboxylate

Benzyl 1-[({4-[(2-aminopyridin-4-yl)oxy]-2,5-difluorophenyl}amino)carbonyl]cyclopropanecarboxylate (1.15 g) was dissolved in tetrahydrofuran (12 ml) under a nitrogen atmosphere. Pyridine (0.424 ml) and phenyl chloroformate (0.657 ml) were added at room temperature, and the mixture was stirred for 20 minutes. A saturated aqueous solution of sodium hydrogencarbonate (36 ml) and hexane (36 ml) were added to the mixture, and the mixture was stirred for 55 minutes. The precipitated solid was collected by filtration. The resultant solid was washed with hexane and dried under aeration and dried by hot air (60° C.) for 5 hours. Water (150 ml) was added to the solid, and the mixture was stirred for 2 hours, and the solid was collected by filtration, and the resultant solid was washed with water. The solid was dried by hot air (60° C.) for 3 days to give the title compound (1.117 g, 76%) as a white solid.

1. stirringthe mixture was stirred for 55 minutes
2. filtrationThe precipitated solid was collected by filtration
3. washThe resultant solid was washed with hexane
4. customdried under aeration
5. customdried by hot air (60° C.) for 5 hours
6. additionWater (150 ml) was added to the solid
7. stirringthe mixture was stirred for 2 hours
8. filtrationthe solid was collected by filtration
9. washthe resultant solid was washed with water
10. customThe solid was dried by hot air (60° C.) for 3 days

ORDレコード

ord-eef348e69af745ceaecdd5406f863899

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08377938B2