反应详情

A solution of 21.0 g (50 mmol) of 4-[3-(acetylamino) cyclopentyl]-α-[(cyclopropylamino)methylene]-2,5-difluoro-β-oxobenzenepropanoic acid, ethyl ester in 250 ml of dry t-butanol was treated with a slurry of 6.2 g (55 mmol) of potassium t-butoxide in 50 ml of dry t-butanol. The resulting suspension was stirred and heated at 65° for 3 hours and then at room temperature overnight. The solvent was removed in vacuo and the residue was dissolved in methylene chloride and washed with 1.0 M hydrochloric acid. After drying (MgSO4) and evaporating the solvent in vacuo, the residue was recrystallized from ethyl acetate/hexane to give 16.5 g of the title compound.

1. temperatureheated at 65° for 3 hours
2. customat room temperature
3. customovernight
4. customThe solvent was removed in vacuo
5. dissolutionthe residue was dissolved in methylene chloride
6. washwashed with 1.0 M hydrochloric acid
7. dry with materialAfter drying (MgSO4)
8. customevaporating the solvent in vacuo
9. customthe residue was recrystallized from ethyl acetate/hexane