Adding a certain compound to certain chemical reactions, such as: 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 35453-19-1, Safety of 5-Amino-2,4,6-triiodoisophthalic acid
Preparation (A); Synthesis of 5-Amino-2,4,6-triiodo-isophthaloyl dichloride (1); 5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol) (commercially available from Aldrich), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA o 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 500C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product.13C NMR (DMSOcZ6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M-H+], expected 593.7; Example 8; N,N’,N”-Tris-[(3(N-2,3-dihydroxypropylcarbamoyl)-2,4,6-triiodo-1-hydroxyl acetamide) phenyl] carbamoyl methyl ethane; Starting material and all other materials were commercially available from Aldrich. a) 5-amino-2,4,6-triiodo-isophtaloyl chloride; 5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA to 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 50C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product.13C NMR (DMSOd6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M-H+], expected 593.7FT-IR (cm”1) 3471, 3372 (NH), 1777 (C=O).
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Reference:
Patent; GE HEALTHCARE AS; WO2007/94683; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com