反応 #63707

反応方程式

3-methoxytetrafluoropropionyl chloride

trifluoroethanol

pyridine

pyridine

→

Trifluoroethyl 3-methoxytetrafluoropropionate

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他Reaction
2. 2
   workup.ADDITIONwas added
3. 3
   ろ過the reaction mixture was filtered
4. 4
   洗浄solids were rinsed with methylene chloride, and filtrates
5. 5
   workup.DISTILLATIONwere distilled

実験手順

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).

出典