反应详情

A solution of rac-2-(3,4-dichloro-phenyl)-2-(tetrahydro-pyran-4-yloxy)-acetamide (278 mg, 0.91 mmol) in toluene (10 mL) was treated with methyl isocyanate (0.08 mL, 1.37 mmol). The resulting solution was heated at reflux for 24 h and then the cooled reaction was concentrated in vacuo. The resulting oil was purified by flash chromatography (Merck Silica gel 60, 230-400 mesh, 20/80 hexanes/ethyl acetate) to afford [1[(3,4-dichloro-phenyl)-(tetrahydro-pyran-4-yloxy)-acetyl]-3-methyl-urea (70 mg, 21% yield) as a colorless oil: EI-HRMS m/e calcd for C15H18N2Cl2O4 (M+) 360.0643, found 360.0865.

1. temperatureThe resulting solution was heated
2. temperatureat reflux for 24 h
3. customthe cooled reaction
4. concentrationwas concentrated in vacuo
5. customThe resulting oil was purified by flash chromatography (Merck Silica gel 60, 230-400 mesh, 20/80 hexanes/ethyl acetate)