反应详情

To a solution of N-[2-[[(2,3-difluorophenyl)methyl]thio]-6-[(1R)-1-[(4R)-2,2-dimethyl-1,3-dioxolan-4-yl]ethoxy]-4-pyrimidinyl]-1-azetidinesulfonamide (the product of step yl) (0.13 g) in DCM (5 mL) was added iron (III) chloride hexahydrate (0.26 g). The reaction mixture was stirred at ambient temperature for 1.5 h, then saturated aqueous sodium bicarbonate (1 mL) was added. The layers were separated and the aqueous material extracted with DCM (×3) and ethyl acetate (×3). The combined organic extracts were washed with saturated aqueous sodium chloride, dried (MgSO4), filtered and evaporated. The residual pale yellow solid was slowly precipitated from DCM, filtered and the resulting material washed with minimal cold DCM (2×1 mL) to afford the title compound as a white powder. Yield: 64 mg,

1. customThe layers were separated
2. extractionthe aqueous material extracted with DCM (×3) and ethyl acetate (×3)
3. washThe combined organic extracts were washed with saturated aqueous sodium chloride
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residual pale yellow solid was slowly precipitated from DCM
8. filtrationfiltered
9. washthe resulting material washed with minimal cold DCM (2×1 mL)