Reaktion #1914816

ord-5e418a0388454984873d7145c34719fc

Reaktionsgleichung

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

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto start reflux
  2. 2
    TemperaturWhile refluxed
  3. 3
    SonstigeAfter the reaction
  4. 4
    Temperaturthe reaction mixture was cooled to room temperature
  5. 5
    workup.STIRRINGthe resulting mixture was well stirred
  6. 6
    FiltrationThereafter, deposits were collected by filtration
  7. 7
    WaschenThe resulting deposits were washed with water
  8. 8
    Waschenby washing with methanol
  9. 9
    SonstigeSubsequently, drying
  10. 10
    Sonstigewas obtained

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07056559B2uspto-grants-2006_06