Carbon Dioxide → 2,2,2-Trifluoroethyl trifluoromethanesulfonate

HRID 1702

반응식

HRID 1702 반응식
[F:1][C:2]([F:8])([F:7])[S:3](Cl)(=[O:5])=[O:4].C(=O)=O.[F:12][C:13]([F:17])([F:16])[CH2:14][OH:15].C(N(CC)CC)C>C(Cl)Cl.CCOCC.CC(O)C>[F:12][C:13]([F:17])([F:16])[CH2:14][O:15][S:3]([C:2]([F:8])([F:7])[F:1])(=[O:5])=[O:4]

참가 물질

8

반응물 4

HCID 280Carbon DioxideHCID 64092,2,2-TrifluoroethanolHCID 8471TriethylamineHCID 79000Trifluoromethanesulfonyl chloride

생성물 1

HCID 803662,2,2-Trifluoroethyl trifluoromethanesulfonate

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 3776Isopropanol용매HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

A solution of trifluoromethanesulfonyl chloride (640 μL, 6 mmol) in CH2Cl2 (5 mL) was cooled under argon to -78° C. (IPA:dry ice bath). 2,2,2-Trifluoroethanol was added (365 μL, 5 mmol) and triethylamine (834 μL, 6 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.

후처리

  1. additionwas added dropwise
  2. stirringthe mixture was stirred at 0° C. for 30 minutes
  3. filtrationThe solids were filtered off
  4. customthe solvent was removed under reduced pressure with the flask
  5. temperaturemaintained at 0° C

출처 및 근거

ORD 기록
ord-9773b48b03f44090887256b458e3e63d
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726172

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