反应详情

温度

50 °C

In a flame-dried reaction flask under a dry nitrogen atmosphere, there was slowly added a solution consisting of 850 mg. of sodium dissolved in 80 ml. of methanol to a slurry of 7.1 g. of 2,3-dichloro-6-methoxyquinoxaline in 60 ml. of methanol at 50° C. over a period of seven hours. The resulting mixture was then heated at 50° C. overnight and finally cooled to room temperature. Upon completion of this step, the spent reaction mixture was concentrated in vacuo and the residue subsequently dissolved in chloroform, followed by washing with water and drying over anhydrous magnesium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, the resulting residue was subsequently chromatographed on a column of 400 ml. of silica gel, followed by elution with toluene. The good fractions were combined and concentrated in vacuo to ultimately afford a white solid consisting of 6.1 g. (88%) of pure 2-chloro-3,6-methoxyquinoxaline. m.p. 79°-81° C.

1. customIn a flame-dried reaction flask under a dry nitrogen atmosphere
2. additionthere was slowly added a solution
3. temperaturefinally cooled to room temperature
4. customUpon completion of this step, the spent reaction mixture
5. concentrationwas concentrated in vacuo
6. dissolutionthe residue subsequently dissolved in chloroform
7. washby washing with water
8. dry with materialdrying over anhydrous magnesium sulfate
9. customAfter removal of the drying agent
10. filtrationby means of filtration
11. customthe solvent by means of evaporation under reduced pressure
12. customthe resulting residue was subsequently chromatographed on a column of 400 ml
13. washof silica gel, followed by elution with toluene
14. concentrationconcentrated in vacuo
15. customto ultimately afford a white solid