反应 #1799

ord-c1eb50330c204669ac80b93517bb8dec

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726172uspto-grants-1998_03