Ethyl Acetate → HCID 178510661, Verbindung

A mixture of 5-cyano-2-(2,6-dichloro-4-trifluoromethylphenyl)imidazole (1.0 g, 0.0033 mol) and bromine (1.9 g, 0.64 ml, 0.13 mol) in 1,1,2,2-tetrachloroethane (20 ml) was stirred and heated at 90° C. for 7 hours. Ethyl acetate (50 ml) was added and the solution was washed with water (50 ml), aqueous sodium metabisulphite solution (50 ml), water (50 ml), dried over anhydrous sodium sulphate and evaporated to dryness. The solid residue was purified by chromatography on silica gel eluting with a mixture of ethyl acetate and petroleum ether (b.p. 60°-80° C.)(3:10) to give 4-bromo-5-cyano-2-(2,6-dichloro-4-trifluoromethylphenyl)imidazole (2.15 g) as a white solid m.p. 270.5°-272° C.

1. washthe solution was washed with water (50 ml), aqueous sodium metabisulphite solution (50 ml), water (50 ml)
2. dry with materialdried over anhydrous sodium sulphate
3. customevaporated to dryness
4. customThe solid residue was purified by chromatography on silica gel eluting with a mixture of ethyl acetate and petroleum ether (b.p. 60°-80° C.)(3:10)

ORD-Eintrag

ord-db3672d63810403e9d4c71056e07b9b2

Quelldatensatz

uspto-grants-1993_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05206257