반응 #1337093

ord-57be91817ee742038bcbfaef9cc66cf7

용매

반응 조건

온도
140°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A flame dried
  2. 2
    기타The flask was fitted with a flame
  3. 3
    기타dried mechanical stirrer
  4. 4
    기타The flask was purged with nitrogen three times
  5. 5
    온도maintained at this temperature for about 24 hours
  6. 6
    온도The reaction mixture was then cooled to 110° C.
  7. 7
    온도maintained at this temperature for 24 hours
  8. 8
    기타The copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 32 hours
  9. 9
    기타to remove any unreacted monomer
  10. 10
    기타at 25° C
  11. 11
    기타at room temperature

실험 절차

A flame dried, 250 mL, round bottom single neck flask was charged with 57.1 grams (0.50 mole) of ε-caprolactone, 51.0 grams (0.50 mole) of p-dioxanone, 4.00 mL (55 mmol) of distilled glycerol, and 0.12 mL (40 μmol) of a 0.33 M stannous octoate solution in toluene. The flask was fitted with a flame dried mechanical stirrer. The flask was purged with nitrogen three times before venting with nitrogen. The reaction mixture was heated to 140° C. and maintained at this temperature for about 24 hours. The reaction mixture was then cooled to 110° C. and maintained at this temperature for 24 hours. The copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 32 hours to remove any unreacted monomer. The copolymer had an inherent viscosity of 0.14 dL/g in HFIP at 25° C. The copolymer was a liquid at room temperature. The molar ratio of PCL/PDS was found to be 53.2/46.8 by proton NMR.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06335383B1uspto-grants-2002_01