反应详情

温度

80 °C

A mixture of methyl 3-carbamimidoyl-4-methylbenzoate (compound 1.9, 400 mg, 1.98 mmol, 1.00 equiv, 95%), 3-bromodihydro-2H-pyran-4(3H)-one (compound 1.10.1, 750 mg, 2.09 mmol, 1.00 equiv), and potassium carbonate (580 mg, 4.20 mmol, 2.00 equiv) in CH3CN (15 mL) was stirred overnight at 80° C. under nitrogen. After cooling to ambient temperature, the reaction mixture was concentrated under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate and washed with 2×10 mL of H2O. The organic phase was dried over (Na2SO4) and concentrated under reduced pressure. The residue was purified using silica gel column chromatography and purified using ethyl acetate/petroleum ether (1/3) to yield 0.21 g (37%) of the title compound as a white solid.

1. temperatureAfter cooling to ambient temperature
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. dissolutionThe residue was dissolved in 50 mL of ethyl acetate
4. washwashed with 2×10 mL of H2O
5. dry with materialThe organic phase was dried over (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified
8. custompurified