反应 #1358983

ord-79d8fae2a5d94f4297f25aa2bf94bab9

反应方程式

CN(C)C=O
DMF
O=C1CCC(=O)N1Br
NBS
CCCCC(CC)COc1ccccc1OCC(CC)CCCC
1b
CCCCC(CC)COc1ccccc1OCC(CC)CCCC
1,2-di(2-ethylhexyloxy)benzene
O=C1CCC(=O)N1Br
NBS
CCCCC(CC)COc1ccc(Br)cc1OCC(CC)CCCC
4-bromo-1,2-di(2-ethylhexyloxy)benzene
收率 96.0%

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 (26.21 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07208122B2uspto-grants-2007_04