反应详情

To a solution of tert-butyl (6R,7R)-6-[(acetylamino)methyl]-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (160 mg) in ethanol (0.5 mL) was added 4.0 M hydrogen chloride-ethyl acetate solution (3 mL), and the mixture was stirred at room temperature for 1.5 hr. The solvent was evaporated under reduced pressure. To the residue was added 1 N aqueous sodium hydroxide solution, and the mixture was extracted twice with ethyl acetate. The combined organic layers were washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was dissolved in ethanol, and a solution of fumaric acid (39.3 mg) in ethanol was added. The solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from ethanol-ethyl acetate to give the title compound (73.5 mg) as colorless crystals.

1. customThe solvent was evaporated under reduced pressure
2. additionTo the residue was added 1 N aqueous sodium hydroxide solution
3. extractionthe mixture was extracted twice with ethyl acetate
4. washThe combined organic layers were washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. dissolutionThe residue was dissolved in ethanol
8. additiona solution of fumaric acid (39.3 mg) in ethanol was added
9. customThe solvent was evaporated under reduced pressure
10. customThe obtained crystals were recrystallized from ethanol-ethyl acetate