反应 #635691

ord-a99fdd18023c4cdf9c7c32264e1d6e44

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

Solid NBS (26.21g, 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 a colorless oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07943062B2uspto-grants-2011_05