Method for preparing 5-amino-2,4,6-triiodoisophthalic acid
A technology of triiodoisophthalic acid and amino, applied in chemical instruments and methods, cyanide reaction preparation, organic compound preparation, etc., can solve the problem of prolonged reaction time, inconvenient production, transportation and storage, and large iodine single substance particle size and other problems, to achieve the effect of simple and convenient production process, easier storage and transportation, and low cost
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0039] Add compound I (30.00g, 165.61mmol) solid and purified water 300.00g to a 500ml three-necked flask equipped with a reflux tube, a thermometer and a mechanical stirrer, add sulfuric acid (6.22g, 62.2mmol) to adjust the pH under magnetic stirring at 25°C 0 to 5, then add elemental iodine (50.44g, 198.74mmol), potassium iodate (21.26g, 99.34mmol), and 30g of methanol to the reaction flask in sequence, raise the temperature to 70°C for reaction, and add sulfuric acid (1.85g , 18.5mmol), 20% (W / W) sodium sulfite aqueous solution (54.25g, 86.08mmol) was added dropwise after 2h until the starch potassium iodide test paper did not turn blue, then concentrated, cooled and crystallized, filtered, and dried to obtain 5-amino 2, 85.19 g of 4,6-triiodoisophthalic acid, the yield was 97.95%, and the purity detected by HPLC was 99.6%.
Embodiment 2
[0041] Add compound I (30.00g, 165.61mmol) solid and purified water 300.00g to a 500ml three-necked flask equipped with a reflux tube, a thermometer and a mechanical stirrer, add sulfuric acid (6.22g, 62.2mmol) to adjust the pH under magnetic stirring at 25°C 0 to 5, then add elemental iodine (50.44g, 198.74mmol) and potassium iodate (21.26g, 99.34mmol) to the reaction flask in turn, raise the temperature to 70°C for reaction, and add sulfuric acid (1.85g, 18.5mmol) dropwise after 7h ), after 2h, 20% (W / W) sodium sulfite aqueous solution (60.24g, 95.58mmol) was added dropwise until the starch potassium iodide test paper did not turn blue, and then concentrated, cooled and crystallized, filtered, and dried to obtain 5-amino 2,4,6 - 88.10 g of triiodoisophthalic acid, lavender gray powdery solid, the yield is 95.39%, and the purity detected by HPLC is 99.5%.
Embodiment 3
[0043]Add compound I (30.00g, 165.61mmol) solid and purified water 300.00g to a 500ml three-necked flask equipped with a reflux tube, a thermometer and a mechanical stirrer, add sulfuric acid (6.22g, 62.2mmol) to adjust the pH under magnetic stirring at 25°C 0 to 5, then add elemental iodine (63.05g, 248.42mmol), potassium iodate (26.58g, 124.20mmol), and 30g methanol to the reaction flask in sequence, raise the temperature to 70°C for reaction, and add sulfuric acid (1.85g , 18.5mmol), 20% (W / W) sodium sulfite aqueous solution (81.65g, 129.56mmol) was added dropwise after 2h until the starch potassium iodide test paper did not turn blue, then concentrated, cooled and crystallized, filtered, and dried to obtain 5-amino 2, 90.46 g of 4,6-triiodoisophthalic acid, gray powdery solid, lavender gray powdery solid, the yield is 92.24%, and the purity detected by HPLC is 99.2%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More