反应详情

温度

100 °C

8.4 g of trifluoromethyl iodide and 5 g of copper powder were stirred with 20 ml of hexamethylphosphoric triamide in a stainless steel laboratory autoclave (Hastelloy) at 120° C. for 2.5 hours. The mixture was filtered with suction over Celite, under nitrogen, to remove the excess copper powder. 1.92 g (5 mmol) of 4-(cis-4-tert-butyl-cyclohexylamino)-6-ethyl-5-iodopyrimidine (Example 1) were added in order to dissolve the trifluoromethyl-copper complex, and the mixture was stirred under nitrogen at 100° C. for 2 hours. After cooling, 200 ml of diethyl ether were added, the precipitated copper salts were filtered off and the filtrate was extracted by stirring with water. The organic phase was dried and concentrated. The product was purified by filtration over a silica gel column (petroleum ether/ethyl acetate 7:3) to give 0.52 g (32% of theory) of product as a colorless oil.

1. filtrationThe mixture was filtered with suction over Celite, under nitrogen
2. customto remove the excess copper powder
3. dissolutionto dissolve the trifluoromethyl-copper complex
4. temperatureAfter cooling
5. filtrationthe precipitated copper salts were filtered off
6. extractionthe filtrate was extracted
7. stirringby stirring with water
8. customThe organic phase was dried
9. concentrationconcentrated
10. filtrationThe product was purified by filtration over a silica gel column (petroleum ether/ethyl acetate 7:3)
11. customto give 0.52 g (32% of theory) of product as a colorless oil