反应 #2353

ord-f9e0a5c87bd84b7d80805188d5773375

溶剂

反应条件

温度
160°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A flame dried
  2. 2
    其他The flask was fitted with a flame
  3. 3
    其他dried mechanical stirrer
  4. 4
    其他The reactor was purged with nitrogen three times
  5. 5
    温度maintained at this temperature for about 18-20 hours
  6. 6
    其他The copolymer was dried under vacuum (0.1 mm Hg) at 110° C. for about 16 hours
  7. 7
    其他to remove any unreacted monomer
  8. 8
    其他at 25° C
  9. 9
    其他at room temperature

实验过程

A flame dried, 250 mL, round bottom single neck flask was charged with 57.1 grams (0.50 mole) of ε-caprolactone, 72.1 grams (0.50 mole) of L-lactide, 4.00 mL (55 mmol) of distilled glycerol, 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 reactor 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 110° C. for about 16 hours to remove any unreacted monomer. The copolymer had an inherent viscosity of 0.14 dL/g in hexafluoroisoproponal (HFIP) at 25° C. The copolymer was a liquid at room temperature. The molar ratio of PCL/PLA was found to be 53.7/46.3 by proton NMR.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728752uspto-grants-1998_03