Triethylamine → HCID 58496687, compound

Participants

Reaction Steps

0.49 ml trifluoroacetic anhydride are added dropwise to a mixture of 1.13 g 5-(3,5-dichloro-phenylsulphonylamino)-naphthalene-1-carboxylic acid amide and 1.07 ml triethylamine in 50 ml methylene chloride while cooling with an ice bath. Then the ice bath is removed and the reaction mixture is stirred for one hour at ambient temperature. In all, another 1.00 ml triethylamine and 0.70 ml trifluoroacetic anhydride are added successively and the reaction mixture is stirred overnight at ambient temperature. For working up the mixture is combined with 50 ml of water. The organic phase is washed with 2 N citric acid solution and saturated sodium hydrogen carbonate solution, dried on magnesium sulphate and evaporated down. The flask residue is chromatographed through a silica gel column with cyclohexane/ethyl acetate (85:15 to 65:35).

Provenance & Evidence