Reaktion #2356

Reaktionsgleichung

ε-caprolactone

p-dioxanone

glycerol

stannous octoate

→

ε-CAPROLACTONE p-DIOXANONE

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA flame dried
2. 2
   SonstigeThe flask was fitted with a flame
3. 3
   Sonstigedried mechanical stirrer
4. 4
   SonstigeThe flask was purged with nitrogen three times
5. 5
   Temperaturmaintained at this temperature for about 24 hours
6. 6
   TemperaturThe reaction mixture was then cooled to 110° C.
7. 7
   Temperaturmaintained at this temperature for 24 hours
8. 8
   SonstigeThe copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 32 hours
9. 9
   Sonstigeto remove any unreacted monomer
10. 10
    Sonstigeat 250° C
11. 11
    Sonstigeat room temperature

Vorschrift

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 0.33M 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 250° 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.

Quelle