反应详情

To a solution of 2-hydroxy-3(S)-{3-(pyridin-3-ylmethanesulfonyl)-2(R)-[2,2,2-trifluoro-1(S)-(4-fluorophenyl)ethylamino]propionylamino} hexanoic acid cyclopropylamide (590 mg, 1 mmol) in methylene chloride, DMP was added slowly. The reaction mixture was stirred at room temperature for 30 min and then a 0.26 M Na2S2O3 in sat. NaHCO3 was added. The reaction mixture was stirred for 20 min. The aqueous layer was extracted with methylene chloride and the combined organic extracts were dried over MgSO4, filtered and concentrated to give 2-oxo-3(S)-{3-(pyridin-3-ylmethanesulfonyl)-2(R)-[2,2,2-trifluoro-1(S)-(4-fluorophenyl)ethylamino]-propionylamino}hexanoic acid cyclopropylamide which was purified by flash column (2% MeOH—CH2Cl2) to give pure product as a yellow solid.

1. stirringThe reaction mixture was stirred for 20 min
2. extractionThe aqueous layer was extracted with methylene chloride
3. dry with materialthe combined organic extracts were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated