Reaktion #167586

Reaktionsgleichung

ethyl (3,3,4,4,4-pentafluoro-butane-1-sulfonyl)-acetate

trifluoro-methanesulfonic acid 2-trifluoromethylsulfanyl-ethyl ester

potassium carbonate

→

Ethyl 2-(3,3,4,4,4-Pentafluoro-butane-1-sulfonyl)-4-trifluoromethylsulfanyl-butyrate

Lösungsmittel

1,2-dimethoxyethane

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate (2×150 mL)
2. 2
   WaschenThe combined organic extracts were washed with brine (200 mL)
3. 3
   Trocknendried over Na2SO4
4. 4
   Einengenconcentrated under reduced pressure
5. 5
   SonstigeThe residue was purified by column chromatography (SiO2, hexanes/CH2Cl2 1:1)
6. 6
   Sonstigeto provide compound II-3 (0.28 g, 37%) as a white solid

Vorschrift

A mixture of ethyl (3,3,4,4,4-pentafluoro-butane-1-sulfonyl)-acetate (J. Fluorine Chem. 1985, 28(4), 425-440) (2.00 g, 6.70 mmol), trifluoro-methanesulfonic acid 2-trifluoromethylsulfanyl-ethyl ester (1.50 g, 5.36 mmol), and potassium carbonate (2.77 g, 5.36 mmol) in 1,2-dimethoxyethane (100 mL) was stirred overnight at room temperature under nitrogen. The reaction mixture was diluted with H2O (200 mL) and extracted with ethyl acetate (2×150 mL). The combined organic extracts were washed with brine (200 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (SiO2, hexanes/CH2Cl2 1:1) to provide compound II-3 (0.28 g, 37%) as a white solid.

Quelle