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A technology of ioversol and chloroethanol, applied in the field of preparation of western medicine compounds, can solve the problems of difficult control of reaction conditions, long reaction time and the like, and achieves the effects of low cost, simple operation and high yield
Inactive Publication Date: 2004-02-25
JIANGSU INST OF NUCLEAR MEDICINE
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Compared with the method reported in US4396598, this method does not involve the use of expensive acetoxyacetyl chloride, but due to the 5-chloroacetamido-N, N'-bis(2,3-dihydroxypropyl)-2 , 4,6-triiodo-1,3-benzenedicarboxamide is insoluble in water, so the step of reacting with anhydrous sodium acetate in this synthetic route is carried out in a heterogeneous system, the reaction time is long, and the reaction conditions are not easy to control
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Embodiment 1
[0015] In a three-necked flask equipped with a stirrer and a reflux condenser, add 50 g (0.064 mol) of 5-chloroacetamido-N, N'-bis(2,3-dihydroxypropyl)-2,4,6- Triiodo-1,3-benzenedicarboxamide, 9g (0.16mol) potassium hydroxide, 250ml water, after all dissolved, add 14g (0.174mol) chloroethanol, stir at 50°C for 15 hours, add 5mol / L hydrochloric acid solution Adjust the pH value of the reaction solution to about 6.0 without purification, directly add 26 g (0.317 mol) of anhydrous sodium acetate to the reaction solution, and add concentrated hydrochloric acid dropwise under stirring to adjust the pH value to 6.5. Heat to reflux, and reflux for 20 hours, during which 5mol / L sodium hydroxide solution is added appropriately to maintain the pH value of the reaction solution at 5.5-6.5.
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Abstract
The present invention relates to a preparation method of X-ray contrast agent ioversol. The method adopts 5-chloroacetamino-N,N'-bis(2,3- dihydroxypropyl)-2,4,6-triodo-1,3-phthalamine and chloroethanol to make them implement alkylation reaction in the presence of inorganic alkali to obtain reaction liquor, said reaction liquor has no need of separation, and the anhydrous sodium acetate can be directly added to make reaction.
Description
technical field [0001] The invention belongs to a preparation method of western medicine compounds, in particular to a preparation method of ioversol, an X-ray non-ionic contrast agent. Background technique [0002] In 1982, U.S. Wanlingke Company successfully developed the non-ionic contrast agent Ioversol (Ioversol, the trade name is Ansheli, Optiray), and the chemical name is N, N'-bis(2,3-dihydroxypropyl) -5-[N-(2-Hydroxyethyl)-glycolamido]-2,4,6-triiodo-1,3-benzenedicarboxamide. Ioversol water solubility is very good, and osmotic pressure is also very low, and chemical property is also more stable, can withstand high temperature sterilization, can be made into injection supply market, can be widely used in blood vessel (applicable to angiography, urinary tract contrast, venography, and contrast-enhanced computer scan), subarachnoid applications (for lumbar, thoracic, and cervical myelography in adults and children, and for pool computer scans after subarachnoid injecti...
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