反应详情

温度

-78 °C

Then, in a nitrogen atmosphere, N-methoxy-N-methyl-anthranilamide (0.62 g, 3.4 mmol), and 3,5-bis(trifluoromethyl)-1-bromobenzene (1.00 g, 3.4 mmol) were dissolved in tetrahydrofuran (20 mL), followed by stirring at −78° C. To the solution, 1.66 mol/L n-butyl lithium (4.11 mL, 6.8 mmol) was gradually added dropwise, followed by stirring for 30 minutes. The reaction was terminated by adding 1 mol/L hydrochloric acid. The reaction solution was extracted with ethyl acetate. The organic layer was washed with a sodium chloride solution and then dried with magnesium sulfate, followed by filtration. The filtrate was concentrated using a rotary evaporator. The residue was purified by recrystallization (hexane). Thus, 3′,5′-bis(trifluoromethyl)-2-aminobenzophenone (1.1 g, 3.3 mmol) was obtained in a yield of 96%.

1. stirringby stirring for 30 minutes
2. customThe reaction was terminated
3. additionby adding 1 mol/L hydrochloric acid
4. extractionThe reaction solution was extracted with ethyl acetate
5. washThe organic layer was washed with a sodium chloride solution
6. dry with materialdried with magnesium sulfate
7. filtrationfollowed by filtration
8. concentrationThe filtrate was concentrated
9. customa rotary evaporator
10. customThe residue was purified by recrystallization (hexane)