反应详情

温度

160 °C

A mixture of 9.0 g (59.9 mmol) of 3-bromoacetophenone, 17.1 g (118 mmol) of N,N′,N″-methylidynetrisformamide, 0.57 g (3.0 mmol) of p-toluenesulfonic acid and 27 g of formamide was stirred at 160° C. for 2 hours. After the reaction mixture was cooled to room temperature, a 5% aqueous solution of caustic soda was added thereto, and the mixture was adjusted to pH 4 with a 5% aqueous hydrochloric acid and extracted with ethyl acetate. The organic layer was washed successively with a saturated aqueous solution of ammonium chloride and saturated brine, then dried and concentrated. The resultant solid residue was recrystallized from a mixture ethanol:water=1:2 to obtain 2.49 g of 4-(3-bromophenyl)pyrimidine.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed successively with a saturated aqueous solution of ammonium chloride and saturated brine
4. customdried
5. concentrationconcentrated
6. customThe resultant solid residue was recrystallized from a mixture ethanol