反应详情

In acetic acid (60 mL) was dissolved methyl 3-(4-{5-[amino(hydroxyimino)methyl]-pyridin-2-yl}phenoxy)-2,2-dimethylpropanoate (5.8 g), acetic anhydride (4 mL) was added to the solution and the mixture was stirred at room temperature for 2 hours. To the residue obtained by concentrating the mixture under reduced pressure were added methanol (300 mL) and tetrahydrofuran (70 mL), and 10% palladium carbon (1.2 g) was added to the mixture under nitrogen atmosphere. The atmosphere of the reaction mixture was made hydrogen atmosphere, and the mixture was stirred at room temperature for 2 hours. After replacing the atmosphere with nitrogen, the mixture was filtered using Celite. The filtrate was concentrated under reduced pressure, ether was added to the obtained residue to pulverize the solid, and the solid was collected by filtration and dried to obtain methyl 3-(4-{5-[amino(imino)methyl]pyridin-2-yl}-phenoxy)-2,2-dimethylpropanoate acetate (6.11 g).

1. additionwas added to the solution
2. customTo the residue obtained
3. concentrationby concentrating the mixture under reduced pressure
4. additionwere added methanol (300 mL) and tetrahydrofuran (70 mL), and 10% palladium carbon (1.2 g)
5. additionwas added to the mixture under nitrogen atmosphere
6. stirringthe mixture was stirred at room temperature for 2 hours
7. filtrationthe mixture was filtered
8. concentrationThe filtrate was concentrated under reduced pressure, ether
9. additionwas added to the obtained residue
10. filtrationthe solid was collected by filtration
11. customdried