2-ethylhexanoic acid tin(II) salt → Poliglecaprone
반응식
[CH2:1]1[O:8][C:6](=[O:7])[CH2:5][O:4][C:2]1=[O:3].C[C@H](O)C(O)=O.[C:15]1(=[O:22])[O:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.CCCCC(C([O-])=O)CC.CCCCC(C([O-])=O)CC.[Sn+2]>>[CH2:1]1[O:8][C:6](=[O:7])[CH2:5][O:4][C:2]1=[O:3].[C:15]1(=[O:22])[O:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1참가 물질
5
반응 조건
- 온도
- 140 °C
실험 절차
16.57 grams (0.143 mol) glycolide (Purac, The Netherlands) was introduced into a three-necked bottle under nitrogen atmosphere and was dried in vacuum at a pressure of less than 0.01 mbar and at 45° C. for at least 8 hours. ε-Caprolactone (Acros, Belgium) was dried over CaH2 and distilled under reduced pressure in a nitrogen atmosphere. 15.76 grams (0.138 mol) ε-caprolactone was added under a nitrogen flow. The ε-caprolactone and the glycolide were mixed at 60° C. 32.27 grams (53.8 mmol) of PEG600 (Merck, dried in vacuum at 0.008 mbar) for at least 8 hours at 90° C.) was added. After this, the mixture was magnetically stirred at a temperature of 140° C. until the mixture became homogeneous. 14.1 mg stannous octoate (Sigma Corp) was added (M/I=8069:1). The reaction was continued during 168 hours at 140° C., where after a complete monomer conversion was observed. The Tg of the pre-polymer was determined by DSC and was −49° C. A PEG-initiated pre-polymer with a glycolide-ε-caprolactone ratio of 51:49 was obtained.