Propylene Glycol → epsilon-Caprolactone p-Dioxanone

HRID 399686

Reaktionsgleichung

Reaktionsgleichung von HRID 399686
[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:9]1[CH2:14][CH2:13][O:12][CH2:11][C:10]1=[O:15].C(O)C(O)C.CCCCC(C([O-])=O)CC.CCCCC(C([O-])=O)CC.[Sn+2]>C1(C)C=CC=CC=1>[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:9]1[CH2:14][CH2:13][O:12][CH2:11][C:10]1=[O:15]

Komponenten

6

Edukt 4

HCID 1030Propylene GlycolHCID 93182-ethylhexanoic acid tin(II) saltHCID 10401epsilon-CAPROLACTONEHCID 18233Dioxanone

Produkt 1

HCID 86748302epsilon-Caprolactone p-Dioxanone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A flame dried, 250 mL, round bottom single neck flask was charged with 57.1 g (0.50 mole) of ε-caprolactone, 51.0 grams (0.50 mole) of p-dioxanone, 3.7 mL (50 mmol) of propylene glycol (USP), and 0.12 mL (34 pmol) 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 and then bath temperature was lowered 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 0.22 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 52.4/47.6 by proton NMR.

Aufarbeitung

  1. customA flame dried
  2. customThe flask was fitted with a flame
  3. customdried mechanical stirrer
  4. customThe flask was purged with nitrogen three times
  5. temperaturemaintained at this temperature for about 24 hours
  6. custombath temperature was lowered to 110° C.
  7. temperaturemaintained at this temperature for 24 hours
  8. customThe copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 32 hours
  9. customto remove any unreacted monomer
  10. customat 25° C
  11. customat room temperature

Quellen und Nachweise

ORD-Eintrag
ord-17153ff91a89443b8ca4625b268cb973
Quelldatensatz
uspto-grants-1998_10
Patentnummer
US05824333

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