Reaktion #2015397

Reaktionsgleichung

3′-[4-(3,4-dichloro-phenyl)-6-trifluoromethyl-pyrimidin-2-yl]-biphenyl-3-sulfonic acid tert-butylamide

TFA

→

title compound

Ausbeute 83.6%

3′-[4-(3,4-Dichloro-phenyl)-6-trifluoromethyl-pyrimidin-2-yl]-biphenyl-3-sulfonic acid amide

Ausbeute 83.6%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturTo a cooled
2. 2
   SonstigeThe mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane
3. 3
   workup.ADDITIONwere added
4. 4
   workup.STIRRINGThe mixture was stirred at room temperature for 1 h
5. 5
   Filtrationthe precipitate was collected by filtration
6. 6
   Sonstigefurther purified by flash chromatography (heptane/ethyl acetate) and crystallization (THF/hexane)

Vorschrift

To a cooled and stirred solution of 3′-[4-(3,4-dichloro-phenyl)-6-trifluoromethyl-pyrimidin-2-yl]-biphenyl-3-sulfonic acid tert-butylamide (0.45 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 and saturated NaHCO3 solution (5 mL), diethyl ether and heptane were added. The mixture was stirred at room temperature for 1 h, the precipitate was collected by filtration and further purified by flash chromatography (heptane/ethyl acetate) and crystallization (THF/hexane) to yield the title compound as a white solid (0.34 g, 72%). MS (ISN) 522.2 [(M−H)−]; mp 241° C.

Quelle