Tributyltin azide → HCID 178439918, compound

Participants

Reaction Steps

4.75 g (12.5 mMol) of 4'-[(2-n-propyl-4-methyl-6-phthalimido-1H-benzimidazol-1-yl)-methyl]-2-cyanobiphenyl are dissolved in 200 ml of absolute toluene and combined with 20.8 g (62.5 mMol) of tributyl tin azide. The reaction mixture is refluxed for 5 days with stirring. Then the solvent is distilled off, the residue is taken up in saline solution and extracted 3 times with 100 ml of ethyl acetate. The combined organic phases are dried over sodium sulphate and evaporated down. The residue is chromatographed on silica gel (particle size: 0.032-0.063 mm) using as eluant first methylene chloride and then methylene chloride/ethanol (50:1, 25:1 and 9:1). The uniform fractions are combined and evaporated down. The residue is triturated with ether/petroleum ether (1:1) and suction filtered.

Provenance & Evidence