Réaction #833518
ord-4648ec85394e4d479980e717bdadd2c8
Équation de réaction
DMF
NBS
1b
1,2-di(2-ethylhexyloxy)benzene
NBS
→
4-bromo-1,2-di(2-ethylhexyloxy)benzene
Rendement 96.0%
Solvants
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1LavageThe organic layer was washed with a saturated LiCl solution and water
- 2SéchageAfter drying with MgSO4 the solvent
- 3Autrewas removed under reduced pressure
- 4workup.DISTILLATIONThe remaining oil was distilled (160° C./0.01 mmHg)
Mode opératoire
Solid NBS (26.21 g, 0.147 mol) was added to an ice cold CH2Cl2 solution (250 mL) of 1b under N2 in the absence of light. Just enough DMF was added (30 mL) to dissolve the NBS. The reaction mixture was allowed to warm to room temperature and then stirred for 12 h. The mixture was then poured into water. The organic layer was washed with a saturated LiCl solution and water. After drying with MgSO4 the solvent was removed under reduced pressure. The remaining oil was distilled (160° C./0.01 mmHg) to yield 4-bromo-1,2-di(2-ethylhexyloxy)benzene (2b) in 96% yield as a colorless oil.