174416-65-0Relevant academic research and scientific papers
Contrast medium of the impurity F synthetic method and its impurity G contrast medium, impurity H and impurity M application in the synthesis of
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, (2019/07/05)
The invention relates to a synthesis method of contrast medium impurities, in particular to a contrast medium impurity F synthetic method and its in the contrast medium impurity G, impurity H and M application in the synthesis of the impurity, which belongs to the field of medical technology. The method is to 5 - nitro - 1, 3 - benzene dicarboxylic acid dimethyl ester (formula 2 compound) and 2, 3 - dihydroxy propylamine as raw materials of formula 3 compound, type 3 compound with hydrogen reduction reaction [...] 4 compound, of formula 4 with a compound obtained by reaction of the impurity F [...] contrast medium. The invention relates to 5 - nitro - 1, 3 - benzene dicarboxylic acid dimethyl ester (formula 2 compound) as the starting material, the synthesis of 5 - amino - N, double-N' - (2, 3 - dihydroxy-propyl) - diiodo - 1, 3 - benzene dicarboxylic amide (formula 1 compounds) and then to of formula 1 as the starting material for the synthesis of impurity G, impurity H and impurity M, for the contrast medium quality control to provide acceptable impurity reference substance.
Novel energy-saving environment-friendly continuous preparation method of iohexol
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Paragraph 0031; 0043; 00045; 0046, (2018/07/28)
The invention relates to a novel energy-saving environment-friendly continuous preparation method of iohexol. The preparation method specifically comprises the following steps: (1) acylation reaction:carrying out a reaction on a compound of a formula [2] with acetic anhydride in an environment of hydrochloric acid to obtain a compound of a formula [3]; (2) transesterification: carrying out a reaction on the compound of the formula [3] with a small-molecule liquid alcohol under an appropriate condition to obtain a compound of a formula [4], (3) alkylation reaction: carrying out a reaction on the compound of the formula [4] with 3-chloro-1,2-propylene glycol under the condition of a mixed solution of methanol and sodium methoxide, carrying out neutralization, filtering and desolvation to obtain an iohexol crude product; (4) purification: purifying the iohexol crude product to obtain an iohexol pure product. The method comprises carrying out the transesterification reaction on the liquidalcohol with 5-acetylamino-2,4,6-triiodo-N,N'-bis(2,3-diacetoxypropyl)-1,3-phthalamide, then carrying out an alkylation reaction with the alkylating reagent 3-chloro-1,2-propylene glycol in a methanol solution of the sodium methoxide, carrying out neutralization by using a methanol solution of hydrochloric acid, carrying out filtering, carrying out desolvation on the obtained filtrate, and thenpurifying the obtained iohexol crude product to obtain the iohexol pure product.
Energy-saving environment-friendly continuous preparation method of iohexol
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Paragraph 0023; 0029; 0031, (2018/07/28)
The invention relates to an energy-saving environment-friendly continuous preparation method of iohexol. The preparation method comprises the following steps: (1) acylation reaction: carrying out a reaction on a compound of a formula [2] with acetic anhydride in an environment of hydrochloric acid to obtain a compound of a formula [3]; (2) transesterification: carrying out a reaction on the compound of the formula [3] with a small-molecule liquid alcohol under an appropriate conditions to obtain a compound of a formula [4]; (3) alkylation reaction: carrying out a reaction on the compound of the formula [4] with and 3-chloro-1,2-propanediol under a condition of a mixed solution of methanol and sodium methoxide to obtain an iohexol crude product; and (4) purification: purifying the iohexol crude product to obtain an iohexol pure product. According to method, the transesterification reaction is carried out on the liquid alcohol with 5-acetylamino-2,4,6-triiodo-N,N'-bis(2,3-diacetoxypropyl)-1,3-phthalamide, then the alkylation reaction is carrred out with the alkylation reagent 3-chloro-1,2-propanediol in a methanol solution of the sodium methoxide, and the obtained iohexol crude product is purified to obtain the pure iohexol product.
PREPARATION OF INTERMEDIATES OF X-RAY CONTRAST AGENTS
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Page/Page column 14, (2014/05/24)
The present invention relates to a process for the preparation of iodinated X-ray contrast agents and in particular to key intermediates thereof. It particularly relates to an improved process for preparation of 5-acetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide (Compound A) or N,N'-bis(2,3-dihydroxypropyl)-5-formamido-2,4,6-triiodoisophthalamide (Compound C), which are intermediates in the industrial preparation of non-ionic X-ray contrast agents. More particularly the invention provides a process for deacylation of the acylated hydroxyl groups of an intermediate compound of Compound A and Compound C.
Acetylation using reduced concentration of acetic acid anhydride for synthesizing non-ionic X-ray contrast agents
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Page/Page column 5, (2011/02/19)
This invention relates to an improved method for the synthesis of 5-acetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide ("Compound A"), an intermediate in the industrial preparation of non-ionic X-ray contrast agents. In particular, it rel
