反应 #1951013

ord-28e86a10ab5f40e7a68ea9e22227d7fa

反应方程式

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
收率 92.9%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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)).

来源

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