반응 #727832

반응 방정식

1-bromo-4-fluoro-2-methyl-benzene

nitronium tetrafluoroborate

→

1-bromo-4-fluoro-2-methyl-5-nitrobenzene

수율 96.4%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도at reflux for 5 h
3. 3
   기타The organic layer was separated
4. 4
   추출the aqueous phase was extracted with dichloromethane (100 mL×3)
5. 5
   건조The combined organic layers were dried over anhydrous Na2SO4
6. 6
   기타evaporated under reduced pressure

실험 절차

To a stirred solution of 1-bromo-4-fluoro-2-methyl-benzene (15.0 g, 79.8 mmol) in dichloromethane (300 mL) was added nitronium tetrafluoroborate (11.7 g, 87.8 mmol) in portions at 0° C. The mixture was heated at reflux for 5 h and was then poured into ice water. The organic layer was separated and the aqueous phase was extracted with dichloromethane (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and evaporated under reduced pressure to give crude 1-bromo-4-fluoro-2-methyl-5-nitrobenzene (18.0 g), which was used directly in the next step.

출처