反应详情

Sodium amalgam (10%, 2 g) was added in small portions to stirred mixture of (1R*,2R*,4S*,5R*)-2′,3′,4′,5′-tetrahydro-4′-[(2RS)-2,3-dihydro-2-methyl-5-trifluoromethoxybenzofuran-7-yl]-1-phenyl-6-phenylsulphonylspiro[8-azabicyclo[3.2.1]octane-2,2′-furan] (Example 18; 160 mg, 0.26 mmol), disodium hydrogen orthophosphate (500 mg), methanol (10 ml) at +5° C. After reaction went to completion, the mixture was quenched with saturated aqueous NaHCO3, decanted and extracted into dichloromethane. The combined organic extracts were dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica gel (dichloromethane:methanol) to give the title compound (83 mg, 67%).

1. customAfter reaction
2. customthe mixture was quenched with saturated aqueous NaHCO3
3. customdecanted
4. extractionextracted into dichloromethane
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by chromatography on silica gel (dichloromethane:methanol)