反应详情

To a solution of 5-[2-(2-chloro-4-hydroxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-1,3-dimethyl-1H-pyridin-2-one (Example 203, step 5, 60 mg) in N,N-dimethylacetamide (2 ml) were added potassium-tert.-butylate (21.5 mg) and 6-chloro-2-trifluoromethyl-nicotinic acid ethyl ester (81 mg). The mixture was stirred at room temperature for 1.5 h. A 0.2 M aqueous LiOH solution (4.79 ml) was added and the mixture was stirred at room temperature for 3 h and then cooled in an ice bath. The mixture was acidified with 1 M aqueous HCl and extracted with ethyl acetate. The organic phase was concentrated to dryness and the product was purified by chromatography ((SiO2, CH2Cl2/MeOH 1:0=>3:1). Off-white solid (22 mg). MS (m/e)=565.2 [M+H+].

1. stirringthe mixture was stirred at room temperature for 3 h
2. temperaturecooled in an ice bath
3. extractionextracted with ethyl acetate
4. concentrationThe organic phase was concentrated to dryness
5. customthe product was purified by chromatography ((SiO2, CH2Cl2/MeOH 1:0=>3:1)