Method for preparing 5-acetamido-2,4,6-triiodo-1,3-benzenedicarboxamides
A technology of phthalamide and acetamido, applied in the field of 5-acetamido-2, can solve problems such as environmental pollution, and achieve the effects of less environmental pollution, high yield and low production cost
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Embodiment 1
[0023] In the 1000 milliliter reaction bottle, add 5-acetamido-2,4,60 grams (0.1 moles) of triiodoisophthalic acid, 8 grams (0.1 moles) of catalyst pyridine, 12.8 grams (0.04 moles) of solid phosgene, 100 ml of 1-butyl-3-methylimidazolium tetrafluoroborate, heated up to 100°C, stirred, and reacted for 4 hours. After the reaction, cooled to below room temperature, 20 ml of ammonia water (25%) was added dropwise while stirring, Raise the temperature to 60°C, stir for 3 hours, after the reaction is complete, cool to room temperature, filter, and discard the filtrate to obtain 48 grams of the product 5-acetamido-2,4,6-triiodo-1,3-benzenedicarboxamide, melting point > 300 °C, yield 80%. The filtrate obtained by filtration was extracted with dichloromethane, and the dichloromethane layer was taken to evaporate the solvent to obtain 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid, which was used for recycling.
Embodiment 2
[0025] In the 1000 milliliter reaction bottle, add 5-acetamido-2,4,60 grams (0.1 moles) of triiodoisophthalic acid, 8 grams (0.1 moles) of catalyst pyridine, 12.8 grams (0.04 moles) of solid phosgene, 100 ml of 1-ethyl-3-methylimidazolium tetrafluoroborate was heated up to 100° C., stirred, and reacted for 4 hours. After the reaction was completed, it was cooled to below room temperature, and 20 ml of ammonia water (25%) was added dropwise while stirring. Raise the temperature to 60°C and stir for 3 hours. After the reaction is complete, cool to room temperature and filter to obtain 48 grams of the product 5-acetylamino-2,4,6-triiodo-1,3-benzenedicarboxamide with a melting point of >300°C. Yield 80%. Extract the filtrate obtained by filtration with dichloromethane, take the dichloromethane layer and evaporate the solvent to obtain 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid, which is used for recycling.
Embodiment 3
[0027] In the 1000 milliliter reaction bottle, add 5-acetamido-2,4,60 grams (0.1 moles) of triiodoisophthalic acid, 16 grams (0.2 moles) of catalyst pyridine, 38.4 grams (0.12 moles) of solid phosgene, 100 ml of 1-butyl-3-methylimidazolium hexafluorophosphate, heated up to 100°C, stirred, and reacted for 4 hours. After the reaction, cooled to below room temperature, 50 ml of ammonia water (25%) was added dropwise with stirring, and heated Stir at 60°C for 3 hours, after the reaction is complete, cool to room temperature, filter, and discard the filtrate to obtain 50 grams of the product 5-acetylamino-2,4,6-triiodo-1,3-phthalamide, melting point > 300°C , yield 83%. Extract the filtrate obtained by filtration with dichloromethane, take the dichloromethane layer and evaporate the solvent to obtain 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid, and the ionic liquid is used for recycling.
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