Preparation of tri-iodo benzene compounds
AssigneeAmersham Health AS
InventorsWilliam Thielking, Einar Odd Ingvoldstad, Trygve Gulbrandsen
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Abstract
The invention provides a process by which ultra low salt content triiodinated aromatic compounds may be isolated from a highly acidic hot triiodination raction reaction medium in a straightforward fashion. The process involves increasing the pH to above 5 a value in the range of 3 to 7 with sodium hydroxide, addition of sodium bisulphite and/or sodium dithionite, addition of seed crystals, cooling slowly, and washing the collected precipitate with water.
Claims6
A process for the preparation of a 2,4,6-triiodinated benzene ring containing compound which comprises iodinating a 2,4,6-unsubstituted benzene ring containing compound with an iodine halide iodinating agent in an aqueous reaction medium at a pH below 4 and precipitating the triiodinated reaction product, characterised in that precipitation of the triiodinated reaction product is effected by:
- adding an aqueous base to the reaction medium while this is at a temperature in the range of 70 to 95° C., thereby to bring the pH of the reaction medium to above 5 a value in the range of 3 to 7;
- adding a reducing agent to the reaction medium while agitating the reaction medium, adding seed crystals of the triiodinated reaction product to the reaction medium;
- cooling the reaction medium to a temperature below 35° C. over a period of 10 to 30 hours, at a cooling rate of 1.5 to 5° C./hour during the period during which precipitation occurs;
- filtering the reaction medium to collect the precipitated triiodinated reaction product;
- and washing the precipitated triiodinated reaction product with from 70 to 200% by weight relative to the weight of the precipitated triiodinated reaction product of water, whereby to yield a product having a salt content of less than 0.1% by weight.
Dependencies are inferred from the claim text.