반응 #1951013

ord-28e86a10ab5f40e7a68ea9e22227d7fa

반응 방정식

CCCCCCCCCCCCCCCOc1ccc(C=O)cc1
p-pentadecanoxybenzaldehyde
[Br-].[Br-].c1ccc([P+](Cc2ccc(C[P+](c3ccccc3)(c3ccccc3)c3ccccc3)cc2)(c2ccccc2)c2ccccc2)cc1
p-xylylenebis(triphenylphosphonium bromide)
CCCCCCCCCCCCCCCOc1ccc(C=Cc2ccc(C=Cc3ccc(OCCCCCCCCCCCCCCC)cc3)cc2)cc1
1,4-bis(4′-pentadecanoxystyryl)benzene
수율 92.9%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A 30-ml four-necked flask was used
  2. 2
    workup.ADDITION6.87 g (35.6 mM) of 28-percent by weight methylate was dropped
  3. 3
    기타at room temperature
  4. 4
    기타(25° C.)
  5. 5
    workup.DISTILLATIONMethanol was distilled out
  6. 6
    workup.ADDITION200 ml of water was added to the residue
  7. 7
    여과Subsequently, the precipitate was filtrated
  8. 8
    세척The resulting precipitate was further washed with water and acetone
  9. 9
    기타by drying

실험 절차

A 30-ml four-necked flask was used, 7.87 g (23.7 mM) of p-pentadecanoxybenzaldehyde synthesized as described above and 8.65 g (11.0 mM) of p-xylylenebis(triphenylphosphonium bromide) were suspended in 100 ml of methanol, and 6.87 g (35.6 mM) of 28-percent by weight methylate was dropped thereto at room temperature (25° C.). Thereafter, aging was performed at a reflux temperature of 65° C. for 3 hours. Methanol was distilled out, and 200 ml of water was added to the residue, followed by agitation. Subsequently, the precipitate was filtrated. The resulting precipitate was further washed with water and acetone, followed by drying, so as to produce 7.49 g of 1,4-bis(4′-pentadecanoxystyryl)benzene isomer mixture (Compound (7)).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07625499B2uspto-grants-2009_12