반응 #63707

반응 방정식

3-methoxytetrafluoropropionyl chloride

trifluoroethanol

pyridine

pyridine

→

Trifluoroethyl 3-methoxytetrafluoropropionate

용매

methylene chloride

반응 조건

후처리

1. 1
   기타Reaction
2. 2
   workup.ADDITIONwas added
3. 3
   여과the reaction mixture was filtered
4. 4
   세척solids were rinsed with methylene chloride, and filtrates
5. 5
   workup.DISTILLATIONwere distilled

실험 절차

Trifluoroethyl 3-methoxytetrafluoropropionate was prepared by reaction of 97.3 g (0.50 mol) of 3-methoxytetrafluoropropionyl chloride, 55.0 g (0.55 mol) of trifluoroethanol, and 39.5 g (0.50 mol) of pyridine in 100 mL methylene chloride. Reaction was extremely slow until the pyridine was added. After having stirred overnight, the reaction mixture was filtered, solids were rinsed with methylene chloride, and filtrates were distilled to give 119.4 g of ester, bp 44°-49° (20 mm, 2.7 kPa). The cloudy product was treated with 2 g of P2O5 and filtered to afford 109.3 g (93%) of the desired ester, pure by GC. IR (CCl4): 2855, 2975, and 3010 (sat'd CH), 1790 (C=O), and 1300-1100 cm-1 (CF, C--O).

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