反应详情

To a solution of 4-bromomethyl-3-trifluoromethyl-benzoic acid ethyl ester 36 (120 mg, 0.386 mmol) in THF (4 mL) and DMF (1 mL) was added K2CO3 (80 mg, 0.579 mmol) and 3-(dimethylamino)pyrrolidine (0.043 mL, 38.6 mg, 0.386 mmol). The resulting mixture was stirred at rt for 4 h. The reaction mixture was poured out in water and extracted twice with ethyl acetate. The combined organic extracts were dried, filtered and concentrated in vacuo. The crude material was purified by chromatography CH2Cl2/MeOH (95/5) to give pure 4-(4-methyl-piperazin-1-ylmethyl)-3-trifluoromethyl-benzoic acid ethyl ester 37 (21 mg, 16%).

1. extractionextracted twice with ethyl acetate
2. customThe combined organic extracts were dried
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by chromatography CH2Cl2/MeOH (95/5)