反応 #1914816

ord-5e418a0388454984873d7145c34719fc

反応方程式

CCC1(CCl)C(C)OC1C
3-chloromethyl-3-ethyl-2,4-dimethyl-oxetane
Oc1ccc(-c2ccc(O)cc2)cc1
4,4′-bisphenol
[K+].[OH-]
potassium hydroxide
CCC1(COc2ccc(-c3ccc(OCC4(CC)C(C)OC4C)cc3)cc2)C(C)OC1C
4,4′-bis[(2,4-dimethyl-3-ethyl-3-oxetanyl)methoxy]biphenyl

溶媒

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to start reflux
  2. 2
    温度While refluxed
  3. 3
    その他After the reaction
  4. 4
    温度the reaction mixture was cooled to room temperature
  5. 5
    workup.STIRRINGthe resulting mixture was well stirred
  6. 6
    ろ過Thereafter, deposits were collected by filtration
  7. 7
    洗浄The resulting deposits were washed with water
  8. 8
    洗浄by washing with methanol
  9. 9
    その他Subsequently, drying
  10. 10
    その他was obtained

実験手順

While stirring, 3-chloromethyl-3-ethyl-2,4-dimethyl-oxetane, 4,4′-bisphenol, and tetrabutylphosphonium bromide were heated to 80° C. An aqueous potassium hydroxide solution was dripped. The resulting mixture was heated to approximately 110° C. to start reflux. While refluxed, the reaction was allowed to proceed over 8 hours. After the reaction, the reaction mixture was cooled to room temperature. Subsequently, pure water was added and the resulting mixture was well stirred. Thereafter, deposits were collected by filtration. The resulting deposits were washed with water, followed by washing with methanol. Subsequently, drying was performed employing a vacuum dryer, whereby a targeted compound was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07056559B2uspto-grants-2006_06