Potassium Carbonate → 2-(3,3,4,4,4-Pentafluoro-butane-1-sulfonyl)-4-trifluoromethylsulfanyl-butyronitrile

A mixture of (3,3,4,4,4-Pentafluoro-butane-1-sulfonyl)-acetonitrile (WO2007/060839) (0.50 g, 1.99 mmol), trifluoro-methanesulfonic acid 2-trifluoromethylsulfanyl-ethyl ester (WO 2007/147888) (0.55 g, 1.99 mmol), and K2CO3 (0.82 g, 5.97 mmol) in 1,2-dimethoxyethane (20 mL) was stirred under nitrogen at room temperature overnight. The reaction mixture was diluted with H2O (50 mL) and extracted with ethyl acetate (2×50 mL). The combined organic extracts were washed with brine (100 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (SiO2, hexanes/EtOAc 19:1) to afford compound II-1 (0.28 g, 37%) as a white solid.

1. extractionextracted with ethyl acetate (2×50 mL)
2. washThe combined organic extracts were washed with brine (100 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography (SiO2, hexanes/EtOAc 19:1)
6. customto afford compound II-1 (0.28 g, 37%) as a white solid

ORD-Eintrag

ord-1bf14432504f4839beb54d5528a54b3b

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08846569B2