HRID2261

反应详情

EQUATION

反应方程式

HRID 2261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A flame dried, 250 mL, round bottom single neck flask was charged with 57.1 g (0.50 mole) of ε-caprolactone, 51.0 grams (0.50 mole) of p-dioxanone, 3.7 mL (50 mmol) of propylene glycol (USP), and 0.12 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 140° C. and maintained at this temperature for about 24 hours and then bath temperature was lowered 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 0.22 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 52.4/47.6 by proton NMR.

WORKUP

后处理

  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. custombath temperature was lowered 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