Acetic Anhydride → 4-Methoxypyridin-2(1H)-one

Temperatur

130 °C

Acetic anhydride (36.3 mL) was added to 4-Methoxy pyridine N-oxide (1.09 g) and the resulting solution was warmed to 130° C. and stirred overnight. After 16 h of stirring, the crude mixture was concentrated on the rotavap. 10 mL of a 1:1 MeOH—H2O solution was added and the resulting mixture was stirred overnight. After 10 h, the mixture was concentrated to a solid. The solid was recrystallized in AcCN, filtered and rinsed with ether.

1. stirringAfter 16 h of stirring
2. concentrationthe crude mixture was concentrated on the rotavap
3. addition10 mL of a 1:1 MeOH—H2O solution was added
4. stirringthe resulting mixture was stirred overnight
5. waitAfter 10 h
6. concentrationthe mixture was concentrated to a solid
7. customThe solid was recrystallized in AcCN
8. filtrationfiltered
9. washrinsed with ether

ORD-Eintrag

ord-031d38de59d54ee5a19afd17f42927a3

Quelldatensatz

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08247556B2