Reaction #1914816

ord-5e418a0388454984873d7145c34719fc

Reaction equation

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

Solvents

Conditions

Temperature
110°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperatureto start reflux
  2. 2
    TemperatureWhile refluxed
  3. 3
    OtherAfter the reaction
  4. 4
    Temperaturethe 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
    WashThe resulting deposits were washed with water
  8. 8
    Washby washing with methanol
  9. 9
    OtherSubsequently, drying
  10. 10
    Otherwas obtained

Procedure

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.

Source

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