反应详情

4-{[(4-Chloro-benzenesulfonyl)-((R)-5,5-difluoro-2-oxo-azepan-3-yl)-amino]-methyl}-3-fluoro-benzoic acid methyl ester (130 mg, 0.26 mmol) was dissolved in THF/MeOH (5 ml) and treated with 1 N NaOH (1.2 ml) for 1.5 h. The reaction mixture was concentrated under reduced pressure diluted using water and extracted with diethyl ether. The aqueous phase was acidified using a 5% KHSO4/10% K2SO4 mixture and extracted with ethyl acetate (3×). The combined organic fractions were washed with brine, dried (Na2SO4), filtered, concentrated under reduced pressure (103 mg). Crude product (50 mg) was purified using preparative RP(C18) chromatography: lyophilisate 22 mg;

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additiondiluted
3. extractionextracted with diethyl ether
4. extractionextracted with ethyl acetate (3×)
5. washThe combined organic fractions were washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure (103 mg)
9. customCrude product (50 mg) was purified