反应详情

A solution of 2.62 g of 4-(cis-4-tert-butylcyclohexylamino)-6-ethyl pyrimidine in 40 ml of trifluoroacetic acid was charged into a reactor for direct fluorination. A stream of a mixture of F2/N2 (1:10 by volume) was passed through the mixture at 15° C. After 0.015 mol of fluorine was passed through, the reaction was flushed with nitrogen in order to remove unconsumed fluorine. The solvent was removed in vacuo and the residue was treated with 50 ml of 2N sodium hydroxide, extracted with diethyl ether, washed with water and dried over MgSO4. After ether evaporation, the product was isolated in 41% yield by column chromatography, eluting with a mixture hexane/ethyl acetate 2:1.

1. customwas passed through the mixture at 15° C
2. customwas flushed with nitrogen in order
3. customto remove unconsumed fluorine
4. customThe solvent was removed in vacuo
5. additionthe residue was treated with 50 ml of 2N sodium hydroxide
6. extractionextracted with diethyl ether
7. washwashed with water
8. dry with materialdried over MgSO4
9. customAfter ether evaporation
10. customthe product was isolated in 41% yield by column chromatography
11. washeluting with a mixture hexane/ethyl acetate 2:1