反应 #2329027

ord-2a1f987398f446249d201859d56748c2

反应方程式

CCCCC(CC)COc1ccc2c(Br)c3cc(OCC(CC)CCCC)ccc3c(Br)c2c1
9,10-dibromo-2,6-di(2-ethylhexyloxy) anthracene
CC(C)[CH2][Al+][CH2]C(C)C.Cc1ccccc1.[H-]
diisobutylaluminum hydride toluene
CCCCC(CC)COc1ccc2c(-c3ccc(C=C(c4ccccc4)c4ccccc4)cc3)c3cc(OCC(CC)CCCC)ccc3c(-c3ccc(C=C(c4ccccc4)c4ccccc4)cc3)c2c1
powder
CCCCC(CC)COc1ccc2c(-c3ccc(C=C(c4ccccc4)c4ccccc4)cc3)c3cc(OCC(CC)CCCC)ccc3c(-c3ccc(C=C(c4ccccc4)c4ccccc4)cc3)c2c1
9,10-bis[4(2,2-diphenylethenyl)phenyl]-2,6-di (2-ethylhexyloxy) anthracene

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONAdded into a 500 ml three-necked flask
  2. 2
    其他equipped with a condenser under a gaseous stream of argon
  3. 3
    温度they were heated
  4. 4
    其他After the completion of the reaction
  5. 5
    过滤the precipitates were filtered
  6. 6
    洗涤washed with methanol 50 ml

实验过程

Added into a 500 ml three-necked flask equipped with a condenser under a gaseous stream of argon were 9,10-dibromo-2,6-di(2-ethylhexyloxy) anthracene 0.6 g (1 mmole), dichlorobis(triphenylphosphine) palladium 0.04 g (5 mole %), diisobutylaluminum hydride/toluene solution 0.1 ml (1 M, 0.1 mmole) and THF 10 ml. After the above-mentioned Grignard reagent was added dropwise to them at room temperature, they were heated and stirred overnight. After the completion of the reaction, the reaction solution was cooled with ice water, the precipitates were filtered and washed with methanol 50 ml followed by acetone 50 ml to give the yellow powder 0.56 g. This was identified as Compound 10 by NMR, IR and field desorption mass spectra measurements (FD-MS) (yield 60%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07670506B1uspto-grants-2010_03