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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Propylene Glycol → epsilon-Caprolactone p-Dioxanone

HRID 2261
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인쇄 미리보기

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HRID 2261 반응식
[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].C(O)C(O)C.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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1030Propylene GlycolHCID 93182-ethylhexanoic acid tin(II) saltHCID 10401epsilon-CAPROLACTONEHCID 18233Dioxanone

생성물 1

HCID 86748302epsilon-Caprolactone p-Dioxanone

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1ec4e94fc0484fc2880ad3dbed35b55d
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05728752

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