反应方程式
[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]参与物
8
反应条件
- 温度
- 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.
后处理
- additionwas added dropwise
- stirringthe mixture was stirred at 0° C. for 30 minutes
- filtrationThe solids were filtered off
- customthe solvent was removed under reduced pressure with the flask
- temperaturemaintained at 0° C
来源与证据
- ORD记录
- ord-c1eb50330c204669ac80b93517bb8dec
- 来源数据集
- uspto-grants-1998_03
- 专利号
- US05726172
关联笔记
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