Reference of 35453-19-1,Some common heterocyclic compound, 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, molecular formula is C8H4I3NO4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
EXAMPLE 3 Methylene chloride (112 g) and tetrabutylammonium bromide (3.23 g; 0.1 moles) were charged in this order into a reactor. 5-Amino-2,4,6-triiodoisophthalic acid (55.9 g; 0.1 moles) and, in about 2 hours, thionyl chloride (57.1 g; 0.479 moles) were added to the mixture while keeping the internal temperature below 36 C. and adjusting the addition rate with the gas emission. At the end of the addition. the reaction mixture was kept under reflux (43 C.) for 27 hours. After cooling to about 20 C., water (60 g) was added in small portions. At about half of the addition, the formation of a crystalline precipitate was observed. After filtration, the resultant product was washed with water (5*50 g) and then dried in oven under vacuum at 50 C. for about 21 hours obtaining 5-amino-2,4,6-triiodoisophthalic acid dichloride (49.99 g; 83.8% yield) practically pure by HPLC analysis and by thin layer chromatography.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Amino-2,4,6-triiodoisophthalic acid, its application will become more common.
Reference:
Patent; Bracco International B.V.; US5856570; (1999); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com