Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Propylene Glycol | HCID 1030 | — |
| Reactant | 2-ethylhexanoic acid tin(II) salt | HCID 9318 | — |
| Reactant | epsilon-CAPROLACTONE | HCID 10401 | — |
| Reactant | Trimethylene carbonate | HCID 123834 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | TMC caprolactone | HCID 11275958 | — |
Reaction Steps
A flame dried, 250 mL, round bottom single neck flask was charged with 102.7 grams (0.90 mole) of ε-caprolactone, 10.2 grams (0.10 mole) of trimethylene carbonate, 2.9 mL (40 mmol) of propylene glycol (USP), and 0.10 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 160° C. and maintained at this temperature for about 18-20 hours. The copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 16 hours to remove any unreacted monomer. The copolymer had an inherent viscosity of 0.25 dL/g in HFIP at 25° C. The copolymer was a viscous liquid at room temperature.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05824333 |
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| Source dataset | uspto-grants-1998_10 |
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| ORD ID | ord-5832ed83ef224ae3bea01c95cc1681b7 |
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| Source note | uspto-grants-1998_10 |
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