反应详情

A mixture of N-({4-[4-(2-{[(3R,3aR,6R,6aR)-6-hydroxy-hexahydrofuro[3,2-b]furan-3-yl]oxy}-6-chloro-3-{[2-(trimethylsilyl)ethoxy]methyl}imidazo[4,5-b]pyridin-5-yl)phenyl]-phenyl}(dimethylamino)oxo-λ6-sulfanylidene)-2,2,2-trifluoroacetamide (22 mg) and trifluoroacetic acid (0.30 mL) in dichloromethane (1.00 mL) is stirred over night at room temperature. The reaction mixture is concentrated in vacuo and the residue is dissolved in methanol. Aqueous Na2CO3 solution (2 N; 60 μL) is added and the mixture is stirred for 1 h. The reaction mixture is filtered and the crude product is purified by preparative HPLC to give the title compound. LC (method 1): tR=0.86 min; Mass spectrum (ESI+): m/z=556 [M+H]+.

1. concentrationThe reaction mixture is concentrated in vacuo
2. dissolutionthe residue is dissolved in methanol
3. additionAqueous Na2CO3 solution (2 N; 60 μL) is added
4. stirringthe mixture is stirred for 1 h
5. filtrationThe reaction mixture is filtered
6. customthe crude product is purified by preparative HPLC