甘油 → epsilon-Caprolactone p-Dioxanone

HRID 2260

反应方程式

HRID 2260 反应方程式
[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:9]1[CH2:14][CH2:13][O:12][CH2:11][C:10]1=[O:15].OCC(CO)O.CCCCC(C([O-])=O)CC.CCCCC(C([O-])=O)CC.[Sn+2]>C1(C)C=CC=CC=1>[C:1]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:9]1[CH2:14][CH2:13][O:12][CH2:11][C:10]1=[O:15]

参与物

6

反应物 4

HCID 753甘油HCID 93182-乙基己酸锡HCID 104016-己内酯HCID 182331,4-二氧六环-2-酮

产物 1

HCID 86748302epsilon-Caprolactone p-Dioxanone

试剂、催化剂与溶剂 1

HCID 1140甲苯溶剂

反应条件

温度
140 °C

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, 51.0 grams (0.50 mole) of p-dioxanone, 4.00 mL (55 mmol) of distilled glycerol, and 0.12 mL (40 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. The reaction mixture was then cooled 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 0.14 dL/g in HFIP at 250° C. The copolymer was a liquid at room temperature. The molar ratio of PCL/PDS was found to be 53.2/46.8 by proton NMR.

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. temperatureThe reaction mixture was then cooled 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 250° C
  11. customat room temperature

来源与证据

ORD记录
ord-2f67cb89cb8f4479a6231aded45cb5b0
来源数据集
uspto-grants-1998_03
专利号
US05728752

关联笔记

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