反应详情

温度

75 °C

A mixture of 4,6-dichloro-5-(4-methylphenyl)pyrimidine (10.0 g), 4-(2-acetoxy-1,1-dimethylethyl)benzenesulfonamide (11.58 g), potassium carbonate (14.45 g) and dimethyl-sulfoxide (50 ml) is stirred at 75° C. (bulk temperature) for 3 hours, and thereto is further added 4-(2-acetoxy-1,1-dimethylethyl)benzenesulfonamide (0.34 g). The mixture is stirred at 70-75° C. for 1.5 hour, and the reaction mixture is cooled, and poured into a mixture of ice (100 g) and conc. hydrochloric acid (60 ml). The mixture is extracted with ethyl acetate, and the organic layer is washed, dried, and concentrated under reduced pressure. The residue is crystallized from a mixture of ethyl acetate and diisopropyl ether to give 4-(2-acetoxy-1,1-dimethylethyl)-N-{6-chloro-5-(4-methylphenyl)pyrimidin-4-yl}benzenesulfonamide (14.97 g) as colorless needles.

1. stirringThe mixture is stirred at 70-75° C. for 1.5 hour
2. temperaturethe reaction mixture is cooled
3. extractionThe mixture is extracted with ethyl acetate
4. washthe organic layer is washed
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe residue is crystallized from a mixture of ethyl acetate and diisopropyl ether