Methanol → HCID 14154315, Verbindung

Temperatur

90 °C

5.8 g of 3-chloro-4-methoxy-2-picoline-N-oxide were dissolved in 8 ml of glacial acetic acid and, while stirring at 90° C., 14 ml of acetic anhydride were added. The mixture was heated at 110°-115° C. for 2 hours and then cooled to 80° C. and 25 ml of methanol were added dropwise. The solvent was then removed by distillation under reduced pressure, and subsequently 20 ml of water and 8 g of sodium hydroxide were added in small portions to the residue, and this mixture was heated to reflux for 2 hours. After cooling, the mixture was extracted with dichloromethane, the solvent was evaporated off, and the residue is induced to crystallize with diethyl ether. Solid, melting point 103°-105° C.

1. temperatureThe mixture was heated at 110°-115° C. for 2 hours
2. temperaturecooled to 80° C.
3. customThe solvent was then removed by distillation under reduced pressure, and subsequently 20 ml of water and 8 g of sodium hydroxide
4. additionwere added in small portions to the residue
5. temperaturethis mixture was heated
6. temperatureto reflux for 2 hours
7. temperatureAfter cooling
8. extractionthe mixture was extracted with dichloromethane
9. customthe solvent was evaporated off
10. customto crystallize with diethyl ether

ORD-Eintrag

ord-d172e5433ce946589a2c92fc98a3f71d

Quelldatensatz

uspto-grants-1989_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04845118