تفاعل #2360

ord-a39ac505275c4aed98cfeb34fa86c787

معادلة التفاعل

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

المذيبات

ظروف التفاعل

درجة الحرارة
160°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA flame dried
  2. 2
    أخرىThe flask was fitted with a flame
  3. 3
    أخرىdried mechanical stirrer
  4. 4
    أخرىThe flask was purged with nitrogen three times
  5. 5
    درجة الحرارةmaintained at this temperature for about 18-20 hours
  6. 6
    أخرىThe copolymer was dried under vacuum (0.1 mm Hg) at 80° C. for about 16 hours
  7. 7
    أخرىto remove any unreacted monomer
  8. 8
    أخرىat 25° C
  9. 9
    أخرىat room temperature

الإجراء التجريبي

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 trimethylene carbonate, 4.4 mL (60mmol) of propylene glycol (USP), and 0.10 mL (34 μmol) of a 0.33M solution of stannous octoate 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 0.20 dL/g in HFIP at 25° C. The copolymer was a viscous liquid at room temperature.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728752uspto-grants-1998_03