反应详情

To a solution of (R)-1-(3-(4-((5-(2-(4-chloro-3-methoxyphenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazol-2-ylthio)methyl)-3,5-difluoro-N-(1-methoxy-1-oxopropan-2-yl)phenylsulfonamido)propyl)-4-aza-1-azoniabicyclo[2.2.2]octane bromide (118 mg, 0.14 mol) in MeCN (2 mL) was added 1N LiOH (0.3 mL). After stirring 1.5 h, the volatiles were removed under educed pressure. The resulting aqueous layer was acidified to pH 0 with 1N HCl and washed with EtOAc (2×10 mL). After extractions, the aqueous layer was neutralized to pH 7 with 1N NaOH and satd NaHCO3, and extracted with DCM/IPA (2:1, v/v, 3×10 mL). The combined extracts were dried (MgSO4), filtered and concentrated under reduced pressure. The residue was triturated in DCM, slurried with Celite and filtered over a pad of Celite to remove any inorganic salts. The DCM layer was concentrated and the residue recrystallized from DCM/Et2O (1:3) to give the title compound (83 mg, 71%) as a white solid.

1. customthe volatiles were removed under educed pressure
2. washwashed with EtOAc (2×10 mL)
3. extractionAfter extractions
4. extractionextracted with DCM/IPA (2:1, v/v, 3×10 mL)
5. dry with materialThe combined extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was triturated in DCM
9. filtrationfiltered over a pad of Celite
10. customto remove any inorganic salts
11. concentrationThe DCM layer was concentrated
12. customthe residue recrystallized from DCM/Et2O (1:3)