Reaktion #800830

Reaktionsgleichung

sodium ethanethiolate

3-chloro-N-(3,5-bistrifluoromethylphenyl)picolinamide

DMF

→

3-ethylsulfanyl-N-(3,5-bistrifluoromethylphenyl)picolinamide

Ausbeute 98.3%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture cooled to room temperature
2. 2
   Filtrationthe precipitated solid was taken by filtration
3. 3
   workup.DISSOLUTIONThe resulting solid was dissolved in ethyl acetate
4. 4
   Extraktionthe mixture was extracted with water and ethyl acetate
5. 5
   TrocknenThe organic layer was dried over anhydrous sodium sulfate
6. 6
   Einengenconcentrated under reduced pressure

Vorschrift

0.89 g of sodium ethanethiolate was added to a mixture of 1.56 g of 3-chloro-N-(3,5-bistrifluoromethylphenyl)picolinamide and 3 mL of DMF, and the mixture was stirred at 60° C. for 2 hours. The reaction mixture cooled to room temperature was poured to water, and the precipitated solid was taken by filtration. The resulting solid was dissolved in ethyl acetate, and the mixture was extracted with water and ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure to obtain 1.64 g of 3-ethylsulfanyl-N-(3,5-bistrifluoromethylphenyl)picolinamide (hereinafter, referred to as Compound of Present Invention 10).

Quelle