反応 #1799

反応方程式

trifluoromethanesulfonyl chloride

dry ice

2,2,2-Trifluoroethanol

triethylamine

→

2,2,2-trifluoroethyltriflate

溶媒

CH2Cl2

IPA

ether

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   workup.STIRRINGthe mixture was stirred at 0° C. for 30 minutes
3. 3
   ろ過The solids were filtered off
4. 4
   その他the solvent was removed under reduced pressure with the flask
5. 5
   温度maintained at 0° C

実験手順

A solution of trifluoromethanesulfonyl chloride (800 uL, 7.5 mmole) in CH2Cl2 (6 mL) was cooled under argon to -60° C. (IPA:dry ice bath). 2,2,2-Trifluoroethanol was added (456 uL, 6 mmol) and triethylamine (1.04 uL, 7.5 mmol) was added dropwise. The reaction was stirred for 1.5 hours then warmed to 0° C. for 1 hour. Anhydrous ether (20 mL) was added and the mixture was stirred at 0° C. for 30 minutes. The solids were filtered off and the solvent was removed under reduced pressure with the flask maintained at 0° C. This afforded the 2,2,2-trifluoroethyltriflate as a yellow oil which was used immediately.

出典