Preparation method of proroiodide

A technology of proammonium iodide and ammonium chloride, which is applied in the field of medicine, can solve the problems of volatile impurities, high toxicity of iodinated reagents, and low yield, and achieve the effects of improving product quality, reducing yield, and low toxicity

Pending Publication Date: 2022-03-22
SUZHOU SIXTH PHARMA PLANT OF JIANGSU WUZHONG PHARMA GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Therefore, the technical problem to be solved in the present invention is to overcome the existence of using iodide reagent toxicity in the prior art proammonium iodide synthesis process, highly volatile and synthetic process impurity on the high side, the defective that yield is low, thereby Provide a kind of preparation method of new promonium iodide

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  • Preparation method of proroiodide
  • Preparation method of proroiodide
  • Preparation method of proroiodide

Examples

Experimental program
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Effect test

Embodiment 1

[0047] The present embodiment provides a kind of preparation route of promonium iodide, and its reaction equation and preparation method are as follows:

[0048]

[0049] (1) Add 310g (1.55mol, 2.0eq) of 30% trimethylamine aqueous solution into a 1L reaction flask, heat up to 40°C, and add dropwise 1,3-dichloro-2-propanol 100g (0.775 mol), the temperature was controlled at 40-45°C, and the reaction was continued at this temperature for 5 hours after dropping.

[0050] After the reaction was completed, it was concentrated to dryness under reduced pressure to obtain an off-white solid. Add 200g of methanol, reflux and dissolve at 82±2°C, cool to 2±2°C for crystallization. After suction filtration, the filter cake was vacuum-dried at 45° C. to obtain 160 g of a white solid (crude ammonium chloride intermediate) with a yield of 84%.

[0051] Recrystallize 160 g of the intermediate ammonium chloride crude product with 240 g of methanol, decolorize with activated carbon, filter...

Embodiment 2

[0055] The present embodiment provides a kind of preparation route of promonium iodide, and its reaction equation and preparation method are as follows:

[0056]

[0057] (1) Add 460g (2.33mol, 3.0eq) of 30% trimethylamine aqueous solution into a 1L reaction flask by weight, raise the temperature to 50°C, and add 100g (0.775mol) of 1,3-dichloro-2-propanol dropwise under stirring. ), the temperature was controlled at 50-55° C., and the dropwise reaction was continued at this temperature for 2 hours.

[0058] After the reaction was completed, it was concentrated to dryness under reduced pressure to obtain an off-white solid. Add 300g of ethanol, reflux and dissolve at 82±2°C, cool to 2±2°C for crystallization. After suction filtration, the filter cake was vacuum-dried at 45° C. to obtain 156 g of a white solid (crude ammonium chloride intermediate), with a yield of 82%.

[0059] 156 g of the intermediate ammonium chloride crude product was recrystallized with 320 g of ethan...

Embodiment 3

[0063] The present embodiment provides a kind of preparation route of promonium iodide, and its reaction equation and preparation method are as follows:

[0064]

[0065] (1) Add 920g (4.66mol, 5eq) of 30% trimethylamine aqueous solution to the 2L reaction flask by weight, raise the temperature to 65°C, add 100g (0.775mol) of 1,3-dichloro-2-propanol dropwise under stirring , the temperature was controlled at 65-70°C, and the mixture was stirred for another 30 minutes after dropping.

[0066] After the reaction was completed, it was concentrated to dryness under reduced pressure to obtain an off-white solid. Add 300g of isopropanol, reflux and dissolve at 82±2°C, cool to 2±2°C for crystallization. After suction filtration, the filter cake was vacuum-dried at 45° C. to obtain 174 g of a white solid (crude ammonium chloride intermediate), with a yield of 91%.

[0067] Recrystallize 174 g of the intermediate ammonium chloride crude product with 350 g of isopropanol, decoloriz...

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Abstract

The invention provides a proroiodide preparation method, which specifically comprises: (1) carrying out a reaction on 1, 3-dichloro-2-propanol and trimethylamine to obtain an intermediate ammonium chloride represented by a formula II; (2) carrying out ion exchange on the intermediate ammonium chloride as shown in the formula II and iodized salt to prepare proroammonium iodide; according to the present invention, the intermediate ammonium chloride is firstly synthesized, and then the intermediate ammonium chloride and the iodized salt are subjected to the ion exchange reaction to prepare the proroiodide, such that the reaction route is reasonable, the condition is mild, the adopted reagent has low toxicity, and the overall reaction yield is high.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a preparation method of promonium iodide. Background technique [0002] Iodine preparations have been used in the field of ophthalmology earlier, and have been used for anti-inflammation and anti-degeneration for a long time, especially in retinal diseases, which have shown good clinical effects. [0003] Iodine preparations first exist in the form of inorganic iodine, such as potassium iodide oral solution. In the 1970s, organic iodine preparations appeared, namely Pronium Iodide. The emergence of organic iodine preparations has improved the adaptability of iodine agents when used in patients with eye diseases, and the side effects have been significantly reduced. Pronium iodide can be injected subconjunctivally or intramuscularly, and gradually decomposes into free iodine after entering the human body, and reaches the aqueous humor and vitreous body through the blood-aqueous humor bar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/08C07C215/18C07C213/04
CPCC07C213/08C07C213/04C07C215/18
Inventor 武卫刘志雨徐兰兰刘宝硕袁双崔恒进
Owner SUZHOU SIXTH PHARMA PLANT OF JIANGSU WUZHONG PHARMA GROUP
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