反应详情

温度

55 °C

1,1-Dimethylethyl 4-{[2-amino-5-methyl-4-(trifluoromethyl)phenyl]amino}-1-piperidine-carboxylate (D58) (2.92 mmol, 1.1 g) was dissolved in 5 ml of tetrahydrofuran and CDI (1,1′-(oxomethanediyl)bis-1H-imidazole) (1.5 eq., 4.4 mmol, 0.71 g) was added at room temperature; the mixture was stirred at 50-60° C. overnight. The mixture was cooled to room temperature and it was partitioned in ethyl acetate/H2O; the two layers were separated and the aqueous phase was extracted with ethyl acetate (2×); the organic phases were combined and washed with citric acid solution (10% aqueous), brine and they were dried over Na2SO4, filtered and the solvent was evaporated to afford the crude compound that was purified by chromatography (ethyl acetate-n-hexane)) to yield the title compound, 900 mg, 81%, M+−H=398.

1. temperatureThe mixture was cooled to room temperature
2. customit was partitioned in ethyl acetate/H2O
3. customthe two layers were separated
4. extractionthe aqueous phase was extracted with ethyl acetate (2×)
5. washwashed with citric acid solution (10% aqueous), brine and they
6. dry with materialwere dried over Na2SO4
7. filtrationfiltered
8. customthe solvent was evaporated
9. customto afford the crude compound that
10. customwas purified by chromatography (ethyl acetate-n-hexane))