反应详情

Methyl 4-(1-{ethoxycarbonyl-[2-(tetrahydropyran-2-yloxy)ethyl]amino}cyclopropyl)benzoate (128 mg) described in Preparation Example 68 was dissolved in methanol (4 mL), 5% hydrogen chloride/methanol was added under ice-cooling, and the mixture was stirred at room temperature for 3.5 hr. The solvent was evaporated from the reaction mixture, N,N-dimethylformamide (4 mL) and potassium carbonate (9 mg) were added, and the mixture was stirred at 140° C. for 6 hr. The reaction mixture was cooled, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (53 mg).

1. temperaturecooling
2. customThe solvent was evaporated from the reaction mixture, N,N-dimethylformamide (4 mL) and potassium carbonate (9 mg)
3. additionwere added
4. stirringthe mixture was stirred at 140° C. for 6 hr
5. temperatureThe reaction mixture was cooled
6. additionwater was added
7. extractionthe mixture was extracted with ethyl acetate
8. washThe organic layer was washed with water and saturated brine
9. customthe solvent was evaporated
10. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)