5-Amino-2,4,6-triiodoisophthalic acid synthesis

Yield:35453-19-1 95.3%

Reaction Conditions:

with potassium iodate;sulfuric acid;potassium iodide in water; pH=< 0.5 at 30 - 75; for 5 h;Reagent/catalyst;Temperature;pH-value;

Steps:

1-9 Example 1
In a 250 mL 3-neck round bottom flask, 5-aminoisophthalic acid (I) (9.060 g, 50 mmol)) solid and 85 ml of purified water were added.Adjust pH The mixture was heated at 30-35 ° C, and KIO3 (11.235 g, 52.5 mmol) was added portionwise to the reaction flask.After reacting at 70-75 ° C for 5 h, it was naturally cooled to room temperature, and the reaction liquid was quenched by adding 20% (w/w) sodium hydrogen sulfite solution (6 g, 11.5 mmol) under stirring, and filtered;And dried to give 5-amino-2,4,6-triiodoisophthalic acid (II) (26.612 g, 47.7 mmol),It was a light brown solid with a yield of 95.3%.By HPLC, the purity is >99.9%, and the maximum single impurity is less than 0.1%, which meets the analytical specifications of industrially produced 5-amino-2,4,6-triiodoisophthalic acid.

References:

Chengdu Xilingyuan Pharmaceutical Co., Ltd.;Gong Jiafu;Sun Jian;Liu Jingfei;Wu Chenglong;Huang Jinkun;Xie Dejian CN110105233, 2019, A Location in patent:Paragraph 0050-0067

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