反应详情

温度

65 °C

A mixture of 5-bromo-2-methylsulfanylpyrimidine-4-carboxylic acid methyl ester (2.3 g), benzenesulfinic acid sodium salt (1.9 g) and dimethyl sulfoxide (35 mL) was treated with bis[copper(I)triflate]benzene complex (3.3 g), and the resulting mixture was stirred at 65° C. for 1.5 hours. The mixture was cooled to 40° C. and filtered through Celite. The filtrate was diluted with ethyl acetate, washed with saturated aqueous sodium hydrogen carbonate solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel, eluting with a mixture of dichloromethane and ethyl acetate (1:0 to 4:1 by volume) to afford the title compound as a pale yellow solid (1.8 g).

1. additionwas treated with bis[copper(I)triflate]benzene complex (3.3 g)
2. temperatureThe mixture was cooled to 40° C.
3. filtrationfiltered through Celite
4. additionThe filtrate was diluted with ethyl acetate
5. washwashed with saturated aqueous sodium hydrogen carbonate solution
6. dry with materialdried over magnesium sulfate
7. customThe solvent was removed under reduced pressure
8. customthe residue purified by column chromatography on silica gel
9. washeluting with a mixture of dichloromethane and ethyl acetate (1:0 to 4:1 by volume)