반응 #2015678

반응 방정식

N-tert-butyl-3-{4-[4-trifluoromethyl-6-(3-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonamide

TFA

→

title compound

수율 70.4%

3-{4-[4-Trifluoromethyl-6-(3-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonamide

수율 70.4%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도To a cooled
2. 2
   기타The mixture was evaporated to dryness
3. 3
   workup.ADDITIONpoured into saturated NaHCO3 solution (20 ml)
4. 4
   추출extracted with ethyl acetate (2×30 ml)
5. 5
   세척The combined organic layers were washed with brine (20 ml)
6. 6
   건조dried (MgSO4)
7. 7
   기타evaporated
8. 8
   기타Further purification
9. 9
   기타by crystallization (diethyl ether)

실험 절차

To a cooled and stirred solution of N-tert-butyl-3-{4-[4-trifluoromethyl-6-(3-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonamide (0.22 g) in dichloromethane (5 ml) was added TFA (5 ml) and the reaction mixture was allowed to stir at room temperature for 15 h. The mixture was evaporated to dryness, poured into saturated NaHCO3 solution (20 ml) and extracted with ethyl acetate (2×30 ml). The combined organic layers were washed with brine (20 ml), dried (MgSO4) and evaporated. Further purification by crystallization (diethyl ether) yielded the title compound as an off-white solid (0.14 g, 65%). MS (ISP) 525.2 [(M+H)+]; mp 244° C.

출처