反応 #1951013

ord-28e86a10ab5f40e7a68ea9e22227d7fa

反応方程式

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
収率 92.9%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A 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
    その他at room temperature
  4. 4
    その他(25° C.)
  5. 5
    workup.DISTILLATIONMethanol was distilled out
  6. 6
    workup.ADDITION200 ml of water was added to the residue
  7. 7
    ろ過Subsequently, the precipitate was filtrated
  8. 8
    洗浄The resulting precipitate was further washed with water and acetone
  9. 9
    その他by drying

実験手順

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)).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07625499B2uspto-grants-2009_12