반응 #2361

ord-8ed745f48d774f70a727a25216a3f78b

반응 방정식

O=C1CCCCCO1
ε-caprolactone
O=C1OCCCO1
trimethylene carbonate
CC(O)CO
propylene glycol
CCCCC(CC)C(=O)[O-].CCCCC(CC)C(=O)[O-].[Sn+2]
stannous octoate
O=C1CCCCCO1.O=C1OCCCO1
ε-CAPROLACTONE TRIMETHYLENE CARBONATE

용매

반응 조건

온도
160°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A flame dried
  2. 2
    기타The flask was fitted with a flame
  3. 3
    기타dried mechanical stirrer
  4. 4
    기타The flask was purged with nitrogen three times
  5. 5
    온도maintained at this temperature for about 18-20 hours
  6. 6
    기타The copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 16 hours
  7. 7
    기타to remove any unreacted monomer
  8. 8
    기타at 25° C
  9. 9
    기타at room temperature

실험 절차

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 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 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728752uspto-grants-1998_03