Glycerol → epsilon-Caprolactone p-Dioxanone

Temperature

140 °C

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.

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. temperatureThe reaction mixture was then cooled 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

ORD record

ord-57be91817ee742038bcbfaef9cc66cf7

Source dataset

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06335383B1