Ethyl Acetate → HCID 178510661, compound

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 elucing 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)
2. dry with materialwater (50 ml), dried over anhydrous sodium sulphate
3. customevaporated to dryness
4. customThe solid residue was purified by chromatography on silica gel elucing with a mixture of ethyl acetate and petroleum ether (b.p. 60°-80° C.)(3:10)

ORD record

ord-f870be53a61e4e6b9d8d27c3157d416c

Source dataset

uspto-grants-1995_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05380865