反应详情

Sodium borohydride (0.077 g) was added portionwise to a suspension of 3-[2-[(4-chlorophenyl)sulphonylamino]ethyl]-5-(4-fluorobenzoyl)benzenepropanoic acid (0.50 g) in ethanol (12 ml), and the resulting solution was stirred at room temperature for 18 hours. 2N hydrochloric acid (5 ml) was added dropwise followed by ethyl acetate (50 ml), and the mixture was stirred for 1 hour. The organic layer was separated, washed with water and dried (MgSO4). The solvent was evaporated and the residue was chromatographed on silica gel. The column was eluted with hexane/ethyl acetate (5:1), followed by hexane/ethyl acetate/acetic acid (50:50:1), gradually increasing the polarity to give a ratio of 10:90:1. The product fractions were combined and evaporated to give the title compound as a gum (0.36 g), Rf 0.45 (SS 15). Found: C,58.58; H,4.71; N,2.65. C24H23ClFNO5S requires C,58.59; H,4.71; N,2.85%.

1. stirringthe mixture was stirred for 1 hour
2. customThe organic layer was separated
3. washwashed with water
4. dry with materialdried (MgSO4)
5. customThe solvent was evaporated
6. customthe residue was chromatographed on silica gel
7. washThe column was eluted with hexane/ethyl acetate (5:1)
8. temperaturegradually increasing the polarity
9. customto give a ratio of 10:90:1
10. customevaporated