反应详情

3-Methyl-2-quinoxalinol (2.84 g, 18 mmol) was dissolved in dry DMF (40 ml) and charged with sodium hydride (55% oil dispersion, 1.0 g, 23 mmol). The resulting solution was cooled under nitrogen to -20° C., whereafter chlorodiethylphosphate (3.3 ml, 23 mmol) was added. The reaction mixture was allowed to reach room temperature, and was then added a -30° C. cold solution of ethyl isocyanoacetate (2.6 g, 23 mmol) and potassium t-butoxide (2.6 g, 23 mmol) in dry DMF (25 ml). The mixture was stirred for 45 min. at ambient temperature, whereafter acetic acid (3 ml) was added. The crystalline precipitate was collected by filtration, rinsed with DMF and water and dried, yielding 2.5 g of the title compound. M.p. 192°-193° C. (Compound 1)

1. additionwas added
2. customto reach room temperature
3. additionwas added
4. filtrationThe crystalline precipitate was collected by filtration
5. washrinsed with DMF and water
6. customdried