Reaktion #2030

ord-a341d33ac8ca4d4dbeafbd8b5790110d

Reaktionsgleichung

N#C[S-].[K+]
potassium thiocyanate
CC(C)=O
acetone
Cc1ccccc1
toluene
C=Cc1ccccc1
styrene
C=Cc1ccc(CSC#N)cc1
4-thiocyanatomethylstyrene

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstige1.5 g of the terpolymer formed in Step II
  2. 2
    Sonstigetaken in a 500 mL flask
  3. 3
    TemperaturThe entire contents of the flask was then heated
  4. 4
    Temperaturto reflux for about 30 hours
  5. 5
    SonstigeThe solvents were evaporated under vacuo
  6. 6
    Sonstigethe residual solids were precipitated from water
  7. 7
    WaschenThe precipitate was washed with methanol
  8. 8
    Sonstigedried
  9. 9
    Sonstigeto yield a white powder of the terpolymer (0.9 g)

Vorschrift

The desired terpolymer of styrene, 4-thiocyanatomethylstyrene, and vinyl benzyl polyethylene glycol was synthesized from the terpolymer of Step II as follows: 1.5 g of the terpolymer formed in Step II was mixed with 350 mL of toluene taken in a 500 mL flask and the contents stirred. To this mixture was added 1.2 g of potassium thiocyanate dissolved in 115 mL of a solvent mixture of DMF and acetone (100/15, v/v). The entire contents of the flask was then heated and allowed to reflux for about 30 hours. The contents were then allowed to cool to room temperature at which time slightly turbid mixture became homogeneous. The solvents were evaporated under vacuo and the residual solids were precipitated from water. The precipitate was washed with methanol and dried to yield a white powder of the terpolymer (0.9 g). The structure of the produced terpolymer was verified by 1H and 13C NMR, and IR spectroscopy.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728431uspto-grants-1998_03