Thionyl Chloride → HCID 87854393, compound

Participants

Reaction Steps

14.5 ml (200 mmol) of thionyl chloride is added in drops at 0° C. within 1 hour to a solution of 34.2 g (200 mmol) of glycine trifluoroacetate in 200 ml of dimethylacetamide. Then, 23.8 g (40 mmol) of 5-amino-2,4,6-triiodoisophthalic acid dichloride (DE 2943777, Schering AG, (priority: Oct. 26, 1979)) is added at 0° C. and stirred for 4 days at room temperature. The reaction mixture is poured into 5liters of ice water and the solid that accumulates is filtered off. For further purification, the filter residue is dissolved in 1000 ml of ethyl acetate, shaken out twice with saturated sodium bicarbonate solution, the organic phase is dried on sodium sulfate, and the solvent is concentrated by evaporation in a vacuum.

Provenance & Evidence