反应详情

温度

60 °C

A 1-liter, four-necked round bottom flask equipped with a mechanical stirrer, condenser, thermowatch and addition funnel was charged with 6-methoxy-4-methyl-2-chloroquinoline (3) (20.75 g, 0.1 moles) and methanol (250 ml). Methanolic sodium methoxide (25%, 108 g, 0.5 moles) was added over 15 minutes. The resulting mixture was heated to reflux and held for 24 hours. Additional methanolic sodium methoxide was added (25%, 42 g, 0.2 moles) and the reaction was refluxed an additional 21 hours. The mixture was cooled to 60° C. and water (200 ml) was added slowly. The slurry was cooled to 10° C., the product isolated by suction filtration, washed with water, and air dried. Yield was 17.9 g (88.2%); mp=58-59° C.; purity by HPLC=100 area %.

1. customA 1-liter, four-necked round bottom flask equipped with a mechanical stirrer, condenser
2. additionthermowatch and addition funnel
3. temperatureThe resulting mixture was heated
4. temperatureto reflux
5. temperaturethe reaction was refluxed an additional 21 hours
6. temperatureThe slurry was cooled to 10° C.
7. customthe product isolated by suction filtration
8. washwashed with water, and air
9. customdried