反应详情

Diethyl dithiophosphate (0.189 mL, 1.13 mmol) was added to a solution (5 mL, 20.00 mmol) of tert-butyl (6R,7R)-7-(4-chloro-3-fluorophenyl)-6-[(3-cyano-2-oxopyridin-1(2H)-yl)methyl]-1,4-oxazepane-4-carboxylate (348 mg, 0.75 mmol) in 4 N hydrogen chloride-ethyl acetate. The reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure. The residue was diluted with saturated aqueous sodium hydrogen carbonate solution (10 mL) and ethyl acetate (10 ml), and di-tert-butyl dicarbonate (0.210 mL, 0.90 mmol) was added. The reaction mixture was stirred at room temperature for 4 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (225 mg, 0.454 mmol, 60.2%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionwas added
3. stirringThe reaction mixture was stirred at room temperature for 4 hr
4. extractionthe mixture was extracted with ethyl acetate
5. washThe extract was washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography