反应详情

温度

0 °C

In 1-neck 250 mL round-bottomed flask, 3-cyano-5-(trifluoromethyl)benzoyl chloride (3.0 g, 1.0 eq.) was dissolved in THF (30 mL, 10 V) at 0° C. Ammonia gas was added and the reaction mixture was stirred for 1-2 h at 0° C. The progress of the reaction was followed by TLC analysis on silica gel with ethyl acetate:hexane (5:5) as mobile phase and visualization with UV, SM Rf=0.10 and Product Rf=0.25. Reaction mixture was quenched into the ice-water slurry (100 mL) and extracted in the ethyl acetate (100 mL×3). Organic layer was washed with brine solution (100 mL) followed by drying using anhydrous sodium sulphate. Organic layer was concentrated under reduced pressure to afford 2.5 g of crude compound as white solid, yield (88%). This crude 3-cyano-5-(trifluoromethyl)benzamide was directly used for next step without purification; Mass: (ES−) 212.95 (M−1).

1. customReaction mixture
2. customwas quenched into the ice-water slurry (100 mL)
3. extractionextracted in the ethyl acetate (100 mL×3)
4. washOrganic layer was washed with brine solution (100 mL)
5. customby drying
6. concentrationOrganic layer was concentrated under reduced pressure