反応 #1530726

反応方程式

DMF

NBS

1b

1,2-di(2-ethylhexyloxy)benzene

NBS

→

4-bromo-1,2-di(2-ethylhexyloxy)benzene

収率 96.0%

溶媒

water

反応条件

後処理

1. 1
   洗浄The organic layer was washed with a saturated LiCl solution and water
2. 2
   乾燥After drying with MgSO4 the solvent
3. 3
   その他was removed under reduced pressure
4. 4
   workup.DISTILLATIONThe remaining oil was distilled (160° C./0.01 mmHg)

実験手順

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 disolve 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.

出典