تفاعل #2076684

معادلة التفاعل

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

TFA

→

title compound

المردود 61.6%

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

المردود 61.6%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةTo a cooled
2. 2
   أخرىThe 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
   ترشيحthe precipitate was collected by filtration
6. 6
   أخرىfurther purified by flash chromatography (heptane/ethyl acetate) and crystallization (dichloromethane/MeOH)

الإجراء التجريبي

To a cooled and stirred solution of 3′-[4-(3-methyl-4-trifluoromethyl-phenyl)-6-trifluoromethyl-pyrimidin-2-yl]-biphenyl-3-sulfonic acid tert-butylamide (0.52 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 (dichloromethane/MeOH) to yield the title compound as an white solid (0.29 g, 54%). MS (ISP) 536.2 [(M−H)−]; mp 205° C.

المصدر