反应详情

温度

20 °C

A solution of 33.9 g of 2-phenylbutyric acid in 340 ml of concentrated sulfuric acid was cooled to -10° C. with stirring. To this solution was added, dropwise, a mixture of 39.4 ml of 70% nitric acid and 170 ml of acetic acid at such a rate that the temperature was maintained below 0° C. The mixture was then warmed to 20° C. over a period of 1 hour and poured into ice water. The off-white solid which formed was separated by filtration, washed with ice water and sucked as dry as possible on the filter. The resultant solid was dissolved in chloroform, a water layer was separated, and the chloroform layer was dried over magnesium sulfate. The solvent was removed under reduced pressure to give a crude solid which was recrystallized from a mixture of hot toluene/hexane to give 2-(4-nitrophenyl)butyric acid.

1. additionTo this solution was added
2. temperaturewas maintained below 0° C
3. customThe off-white solid which formed
4. customwas separated by filtration
5. washwashed with ice water
6. customas dry as possible on the filter
7. dissolutionThe resultant solid was dissolved in chloroform
8. customa water layer was separated
9. dry with materialthe chloroform layer was dried over magnesium sulfate
10. customThe solvent was removed under reduced pressure
11. customto give a crude solid which
12. customwas recrystallized from a mixture of hot toluene/hexane