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With caesium carbonate; In DMF (N,N-dimethyl-formamide); at 25.0℃; for 2.0h;
A mixture of <strong>[31570-97-5]5-hydroxyquinolin-2-(1H)-one</strong> (0.05 g, 0.31 mmol, prepared as described in Shono, T., Matsumura, Y., Kashimura, S., J. Org. Chem. 1981, 46, 3719.), 4,6-difluoropyrimidine (0.036 mL, 0.31 mmol, ABCR) and cesium carbonate (0.2 g, 0.62 mmol) in DMF (5 mL) was stirred at 25° C. for 2 h. The reaction mixture was then diluted with H2O (25 mL). The resulting off-white precipitate was collected by filtration and dried under vacuo to give the title compound. MS (ESI, pos. ion.) m/z: 258 (M+1).
With potassium carbonate; In water; dimethyl sulfoxide; toluene;
EXAMPLE 92 5-(4-Phenylmercapto-butoxy)-carbostyril 49 gm of 4-phenylmercapto-butyl bromide were added to a mixture of 32.3 gm of <strong>[31570-97-5]5-hydroxy-carbostyril</strong>, 30 gm of potassium carbonate and 650 ml of dimethylsulfoxide which had been dried over a molecular sieve. The mixture was stirred for 20 hours at 25° C., diluted with 3 liters of water, and the crystallized reaction product was suction-filtered off. M.p.: 185°-187° C. (from toluene) Yield: 45.0 gm (70percent of theory).
With sodium hydroxide; In ethanol; water; acetone;
REFERENCE EXAMPLE 1 0.6 g of sodium hydroxide was dissolved in 40 ml of water, and 2.0 g of <strong>[31570-97-5]5-hydroxycarbostyril</strong> and 2.5 g of epichlorohydrin were added to the solution. The mixture was stirred at a temperature of from 60° to 70°C for 5 hours followed by cooling to precipitate the product. The precipitated crystals were washed with water, dissolved in ethanol and then subjected to thin layer chromatography using acetone as an elude to obtain two spots having a Rf value of 0.58 and 0.65, respectively, The spot having a Rf value of 0.58 was extracted with ethanol and crystallized to obtain 5-(2,3-epoxy)propoxycarbostyril which was used as the starting material in Examples 1 and 2.
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