反応 #2329027

ord-2a1f987398f446249d201859d56748c2

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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%).

出典

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