反应详情

温度

60 °C

A mixture of the compound (1.3 g) obtained in step 1, benzyl trans-4-aminocyclohexanecarboxylate monohydrochloride (1.1 g), potassium carbonate (0.88 g) and DMF (30 mL) was stirred at 60° C. for 6 hr. The mixture was diluted with water, and extracted with ethyl acetate. The extract was washed with water and saturated brine, dried and concentrated under reduced pressure. The residue was separated and purified by silica gel column chromatography (solvent gradient; 0→25% ethyl acetate/hexane) to give benzyl trans-4-(5,5-dimethyl-2,4-dioxo-1,3-oxazolidin-3-yl)cyclohexanecarboxylate (1.2 g, 81%) as a white powder.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with water and saturated brine
3. customdried
4. concentrationconcentrated under reduced pressure
5. customThe residue was separated
6. custompurified by silica gel column chromatography (solvent gradient; 0→25% ethyl acetate/hexane)