反应详情

Into a solution of 1.6 g of dl-5-chloro-6-ethyl-4-(α-ethyl-4-hydroxybenzyl)aminopyrimidine sodium salt dissolved in 30 ml of N,N-dimethylformamide was gradually bubbled about 2.2 g of tetrafluoroethylene at 80° C. under nitrogen atmosphere while stirring. After completion of the bubbling, the mixture was stirred for 2 hours, and the reaction mixture was charged into water and separated oily product was extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and ethyl acetate was distilled off under reduced pressure. The oily product obtained was isolated by column chromatography (Wako Gel C-200, trade name, eluted with toluene:ethyl acetate=7:1) to give 0.6 g of the desired product as pale yellow liquid.

1. customat 80° C.
2. stirringAfter completion of the bubbling, the mixture was stirred for 2 hours
3. customseparated oily product
4. extractionwas extracted with ethyl acetate
5. washThe extract was washed with water
6. dry with materialdried over anhydrous sodium sulfate and ethyl acetate
7. distillationwas distilled off under reduced pressure
8. customThe oily product obtained