Reaktion #993477

Reaktionsgleichung

3′-[4-methyl-6-(6-trifluoromethyl-pyridin-3-yl)-pyrimidin-2-yl]-biphenyl-3-sulfonic acid tert-butylamide

TFA

→

title compound

Ausbeute 37.8%

3′-[4-Methyl-6-(6-trifluoromethyl-pyridin-3-yl)-pyrimidin-2-yl]-biphenyl-3-sulfonic acid amide

Ausbeute 37.8%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturTo a cooled
2. 2
   SonstigeThe mixture was evaporated to dryness
3. 3
   workup.ADDITIONpoured into 2N Na2CO3 solution (25 ml)
4. 4
   Extraktionextracted with ethyl acetate (3×50 ml)
5. 5
   WaschenThe combined organic layers were washed with brine (50 ml)
6. 6
   Trocknendried (MgSO4)
7. 7
   Sonstigeevaporated
8. 8
   SonstigeFurther purification
9. 9
   Sonstigeby crystallization (ethyl acetate/heptane)

Vorschrift

To a cooled and stirred solution of 3′-[4-methyl-6-(6-trifluoromethyl-pyridin-3-yl)-pyrimidin-2-yl]-biphenyl-3-sulfonic acid tert-butylamide (0.24 g) in dichloromethane (6 ml) was added TFA (6 ml) and the reaction mixture was allowed to stir at room temperature for 15 h. The mixture was evaporated to dryness, poured into 2N Na2CO3 solution (25 ml) and extracted with ethyl acetate (3×50 ml). The combined organic layers were washed with brine (50 ml), dried (MgSO4) and evaporated. Further purification by crystallization (ethyl acetate/heptane) yielded the title compound as a white solid (0.081 g, 34%). MS (ISP) 471.2 [(M+H)+]; mp 220° C.

Quelle