반응 #2168941

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trimethylene carbonate

l-lactide

1,6-hexanediol

→

Trimethylene Carbonate l-Lactide

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후처리

1. 1
   기타In a 100 mL reaction flask
2. 2
   기타fitted with mechanical stirrer and argon inlet
3. 3
   기타The flask was evacuated
4. 4
   workup.ADDITIONfilled with argon several times
5. 5
   기타immersed in an oil bath at 160° C.
6. 6
   workup.ADDITION, the polymerization catalyst, 25 μL of 0.02M solution of tin(II) octoate in toluene, was added via syringe
7. 7
   workup.STIRRINGThe mixture was stirred at 160° C. for 4 hrs
8. 8
   기타, then the polymer was removed from the flask
9. 9
   workup.DISSOLUTIONdissolved in tetrahydrofuran (450 mL)
10. 10
    기타precipitated into methanol (1200 mL) in a blender
11. 11
    workup.STIRRINGThe precipitated polymer was stirred with additional methanol (400 mL) in the blender
12. 12
    여과filtered
13. 13
    기타dried in the vacuum oven at 50° C

실험 절차

In a 100 mL reaction flask fitted with mechanical stirrer and argon inlet were combined trimethylene carbonate (51.45 g, 504 mmol), l-lactide (8.07 g, 56 mmol), and 1,6-hexanediol (47 mg, 0.40 mmol). The flask was evacuated and filled with argon several times, immersed in an oil bath at 160° C. and stirring was initiated. After 10 mins., the polymerization catalyst, 25 μL of 0.02M solution of tin(II) octoate in toluene, was added via syringe. The mixture was stirred at 160° C. for 4 hrs., then the polymer was removed from the flask, dissolved in tetrahydrofuran (450 mL), and precipitated into methanol (1200 mL) in a blender. The precipitated polymer was stirred with additional methanol (400 mL) in the blender, filtered, and dried in the vacuum oven at 50° C. Yield: 43.8 g (74%). Weight average molecular weight=120,000 (polydispersity 1.5). Proton NMR (400 MHz) shows a final composition of 80% trimethylene carbonate units and 20% lactic acid units (theoretical 82% and 18%, respectively). This polymer is especially useful as a coating polymer.

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