反应详情

温度

60 °C

1-Methylcyclopropyl 4-nitro-phenyl carbonate (58 mg) is added to a mixture of 5-(1-methanesulfonyl-1,2,3,6-tetrahydro-pyridin-4-yl)-dispiro[2,3-dihydrofuro[2,3-c]pyridine-2,1′-cyclobutane-3′,4″-piperidine] (HCl salt; 66 mg), triethylamine (65 μL), and tetrahydrofuran (5 mL) at room temperature. The solution is stirred at 60° C. overnight. Water is added and the resulting mixture is extracted with ethyl acetate. The combined extracts are dried (Na2SO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 4:1→1:4) to give the title compound. LC (method 1): tR=1.02 min; Mass spectrum (ESI+): m/z=488 [M+H]+.

1. extractionthe resulting mixture is extracted with ethyl acetate
2. dry with materialThe combined extracts are dried (Na2SO4)
3. concentrationconcentrated
4. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 4:1→1:4)