Reaktion #2353

ord-f9e0a5c87bd84b7d80805188d5773375

Reaktionsgleichung

O=C1CCCCCO1
ε-caprolactone
C[C@@H]1OC(=O)[C@H](C)OC1=O
L-lactide
OCC(O)CO
glycerol
CCCCC(CC)C(=O)[O-].CCCCC(CC)C(=O)[O-].[Sn+2]
stannous octoate
C[C@@H]1OC(=O)[C@H](C)OC1=O.O=C1CCCCCO1
ε-CAPROLACTONE L-LACTIDE

Lösungsmittel

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA flame dried
  2. 2
    SonstigeThe flask was fitted with a flame
  3. 3
    Sonstigedried mechanical stirrer
  4. 4
    SonstigeThe reactor was purged with nitrogen three times
  5. 5
    Temperaturmaintained at this temperature for about 18-20 hours
  6. 6
    SonstigeThe copolymer was dried under vacuum (0.1 mm Hg) at 110° C. for about 16 hours
  7. 7
    Sonstigeto remove any unreacted monomer
  8. 8
    Sonstigeat 25° C
  9. 9
    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, 72.1 grams (0.50 mole) of L-lactide, 4.00 mL (55 mmol) of distilled glycerol, and 0.10 mL (34 μmol) of a 0.33M stannous octoate solution in toluene. The flask was fitted with a flame dried mechanical stirrer. The reactor was purged with nitrogen three times before venting with nitrogen. The reaction mixture was heated to 160° C. and maintained at this temperature for about 18-20 hours. The copolymer was dried under vacuum (0.1 mm Hg) at 110° C. for about 16 hours to remove any unreacted monomer. The copolymer had an inherent viscosity of 0.14 dL/g in hexafluoroisoproponal (HFIP) at 25° C. The copolymer was a liquid at room temperature. The molar ratio of PCL/PLA was found to be 53.7/46.3 by proton NMR.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05728752uspto-grants-1998_03