反应详情

1.0 g of triethylamine and 2.2 g of 2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamine were added to 1.8 g of 4,5-dichloro-2,6-dimethylpyrimidine dissolved in 50 ml of toluene. The mixture was heated under reflux, whilst stirring, for 5 hours. At the end of this time, the reaction product was washed with water and dried over anhydrous sodium sulfate. Toluene was then removed by distillation under reduced pressure, and the oily product obtained was subjected to column chromatography (Wakogel C-200, eluted with a 2:1 by volume mixture of toluene and etyl acetate) to isolate the product. The crystals obtained were recrystallized from hexane, to give 2.0 g of the title compound as colorless granular crystals melting at 61°-63° C.

1. temperatureThe mixture was heated
2. temperatureunder reflux
3. washAt the end of this time, the reaction product was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customToluene was then removed by distillation under reduced pressure
6. customthe oily product obtained
7. washeluted with a 2:1 by volume mixture of toluene and etyl acetate)
8. customto isolate the product
9. customThe crystals obtained
10. customwere recrystallized from hexane