Novel method for preparing iomeprol
A technology of iomeprol and a new method, applied in the field of preparing iomeprol, can solve problems such as high cost, increased environmental protection cost, and complicated handling, and achieve the effects of stable quality, low cost and high yield
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[0035] The preparation method of iomeprol provided in the examples of the present invention uses the compound 5-aminoisophthalic acid as a raw material to carry out N-methylation reaction, esterification reaction, amidation reaction, iodination reaction, chloroacetylation reaction, hydroxylation Reaction, make iomeprol;
[0036] The reaction scheme is as follows:
[0037]
[0038] Such as figure 1 As shown, the preparation method of iomeprol provided by the embodiments of the present invention includes:
[0039] S101: N-methylation reaction: the compound 5-aminoisophthalic acid of formula (2) and 38% formaldehyde carry out N-methylation reaction, with chloroform as solvent, concentrated sulfuric acid as catalyst, the compound of formula (2): The molar ratio of formaldehyde: chloroform: sulfuric acid is controlled to be 1:9:9:0.8. In a clean four-necked reaction flask equipped with stirring and reflux condenser, add the compound of formula (2) and dissolve it in chloroform...
Embodiment 1
[0050] a) Add 215g of chloroform into a clean 500ml reaction flask, add 36.2g of 5-aminoisophthalic acid under stirring, add 15.6g of concentrated sulfuric acid dropwise below 50°C, heat up to 50-60°C after dropping, and Add 142g of 38% formaldehyde solution dropwise at this temperature, react at this temperature for 5-7 hours after dropping, then lower the temperature and depressurize to evaporate chloroform, add 126g of ice water and stir for 5 hours, filter, add methanol and filter cake Recrystallized with water, filtered and dried to obtain 33.4 g of white solid, 85% yield, 5-methylaminoisophthalic acid (calculated as 5-aminoisophthalic acid);
[0051] b) Add 60g of methanol into a clean 250ml reaction flask, add 19.5g of 5-methylaminoisophthalic acid and 3g of concentrated sulfuric acid under stirring; after heating and reflux for 7 hours, cool down to below 10°C to crystallize for 9 hours, filter and freeze Wash the filter cake with water, and dry to obtain 20.9 g of whi...
Embodiment 2
[0057] a) Add 100kg of chloroform into a clean 250L reaction kettle, add 18kg of 5-aminoisophthalic acid under stirring, add 8kg of concentrated sulfuric acid dropwise below 50°C, and raise the temperature to 50-60°C after dripping. Add 72kg of 38% formaldehyde solution dropwise within the temperature range, react at this temperature for 7 hours after dropping, lower the temperature and reduce pressure to evaporate chloroform, add 60kg of ice water and stir for 6 hours, filter, add methanol and water to the filter cake for recrystallization , filter and dry to get 16.8kg5-methylaminoisophthalic acid (yield 86%);
[0058] b) Add 60kg of methanol into a clean 250L reaction kettle, add 19.5kg of 5-methylaminoisophthalic acid and 3kg of concentrated sulfuric acid under stirring; after heating to reflux for 9 hours, cool down to below 10°C to crystallize for 11 hours, filter and freeze Wash the filter cake with water, and dry to obtain 21kg of 5-methylaminoisophthalic acid dimethyl...
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