반응 #47600

반응 방정식

triflic anhydride

2,2-difluoroethanol

triethylamine

→

trifluoro-methanesulfonic acid 2,2-difluoro-ethyl ester

수율 75.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   기타In a flask under argon was placed
2. 2
   workup.ADDITIONAfter the addition
3. 3
   농축concentrated in vacuo
4. 4
   workup.DISTILLATIONThis material was distilled at 60° C.

실험 절차

In a flask under argon was placed triflic anhydride (10.22 mL, 61 mmol) and dichloromethane (10 mL) and it was cooled to −70° C. To this cooled mixture was added slowly a solution of 2,2-difluoroethanol (5.00 g, 61 mmol) and triethylamine (8.5 mL, 61 mmol) in dichloromethane (10 mL). After the addition was complete, the mixture was warmed to 25° C. and then concentrated in vacuo. This material was distilled at 60° C. and 50 mm Hg which afforded trifluoro-methanesulfonic acid 2,2-difluoro-ethyl ester (9.74 g, 75%) as a colorless oil.

출처