反応 #2030

ord-a341d33ac8ca4d4dbeafbd8b5790110d

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他1.5 g of the terpolymer formed in Step II
  2. 2
    その他taken in a 500 mL flask
  3. 3
    温度The entire contents of the flask was then heated
  4. 4
    温度to reflux for about 30 hours
  5. 5
    その他The solvents were evaporated under vacuo
  6. 6
    その他the residual solids were precipitated from water
  7. 7
    洗浄The precipitate was washed with methanol
  8. 8
    その他dried
  9. 9
    その他to yield a white powder of the terpolymer (0.9 g)

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728431uspto-grants-1998_03