Reaktion #81542

Reaktionsgleichung

caprolactone

caprolactone

Caprolactone

→

Caprolactone Acrylate

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeconjugates capped by acrylation
2. 2
   workup.DISTILLATION150 ml of the toluene were distilled off at 110° C.
3. 3
   Sonstigeto remove water
4. 4
   workup.ADDITION8.5 mls of triethylamine were added
5. 5
   Sonstigethe reaction mixture was precipitated in hexane
6. 6
   SonstigeThe hexane precipitate was recovered on a medium Buchner funnel
7. 7
   workup.DISSOLUTIONdissolved in THF (tetrahydrofuran) at 40° C. on a water bath
8. 8
   SonstigeThe collected filtrate was evaporated to dryness on a rotary evaporator
9. 9
   Sonstigeplaced under vacuum overnight

Vorschrift

This example illustrates the synthesis of PEG-caprolactone conjugates capped by acrylation. 90 g of the PEG-caprolactone synthesized in Example 9 were added to a 1000 ml three-neck flask. 900 mL of anhydrous toluene were added, and 150 ml of the toluene were distilled off at 110° C. to remove water. The solution was cooled to 60° C. and 8.5 mls of triethylamine were added, followed by 4.8 ml of acryloyl chloride, dropwise from a piper. After 15 minutes, the reaction mixture was precipitated in hexane. The hexane precipitate was recovered on a medium Buchner funnel and dissolved in THF (tetrahydrofuran) at 40° C. on a water bath. The THF solution was then passed through 90 gm of alumina, prewetted with THF, on a Buchner funnel. The collected filtrate was evaporated to dryness on a rotary evaporator and placed under vacuum overnight. Yield was about 65 gm.

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