反应详情

温度

-78 °C

70% Nitric acid (3.16 mL) was added dropwise to a suspension of trifluoromethanesulfonic acid (9.34 mL, 105.6 mmol) in dichloromethane (250 mL). The suspension was-cooled in a dry ice-acetone bath and a solution of 4-benzyl-benzoic acid (10.19 g, 48 mmol) in dichloromethane (50 mL) was added dropwise. The mixture was stirred for about 2 hours at −78° C. and an additional 2 hours at room temperature. The reaction mixture was poured into crushed ice. The separated organic layer was washed with dichloromethane (2×) and the combined organic layers were dried over (Na2SO4), and solvents were evaporated. Recrystallization of the crude product from methanol/ethyl acetate gave 4-(4-nitrobenzyl)-benzoic acid (9.27 g, 58%) as a yellow solid.

1. temperatureThe suspension was-cooled in a dry ice-acetone bath
2. additionThe reaction mixture was poured
3. custominto crushed ice
4. washThe separated organic layer was washed with dichloromethane (2×)
5. dry with materialthe combined organic layers were dried over (Na2SO4), and solvents
6. customwere evaporated
7. customRecrystallization of the crude product from methanol/ethyl acetate