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Oxapium iodide preparation method

A technology of oxalammonium iodide and phenyl, which is applied in the field of preparation of oxalammonium iodide, can solve the problems of inability to adapt to industrial production, great harm to the human body, and difficulty in obtaining it, and achieves short process reaction time, convenient operation, and low toxicity. Effect

Active Publication Date: 2017-04-12
HEFEI PINGGUANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In foreign countries, only Japanese patents JP: 56-25175, JP: 56-30971 and JP: 56-71089 have been described, and their common characteristics are all based on 2-cyclohexyl-2-phenyl-4-p-toluenesulfonate Acyloxy-1,3-dioxolane is used as the starting material, which is not easy to obtain. At the same time, column chromatography technology is required to separate the intermediate during the purification process, which cannot meet the requirements of industrial production
[0004] Disclosed in Chinese patent CN101121708B is a preparation method of oxalanium iodide, using cyclohexyl phenyl ketone and 3-chloro-1,2 propanediol as reaction raw materials, raw materials are cheap and easy to get, but 3-chloro-1,2 propanediol It is a flammable, highly toxic and suspected carcinogen, which is very harmful to the human body

Method used

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preparation example Construction

[0025] refer to figure 1 , the preparation method of a kind of oxalamium iodide that the present invention proposes, comprises the steps:

[0026] S1. Preparation of 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol: mix cyclohexyl phenyl ketone, glycerin, Amberlyst-15 exchange resin, and color-changing silica gel, heat up, and keep stirring , filter, take the filtrate and add saturated aqueous sodium bicarbonate solution to wash, let the organic layer stand still, dry, and distill under reduced pressure to obtain material A; purify material A and dry to obtain 2-phenyl-2-cyclohexyl-4-methanol-1 ,3-dioxin;

[0027] S2. Preparation of 2-phenyl-2-cyclohexyl-4-piperidinylmethyl-1,3-dioxol: take piperidine, pass through an inert gas, and sequentially add 2-phenyl-2- Cyclohexyl-4-methanol-1,3-dioxol, catalyst TiO 2 / Pt mixing, adjust the temperature, irradiate with a high-pressure mercury lamp, stir continuously during the irradiation process, filter, take the filtrate and concentrate...

Embodiment 1

[0031] A preparation method for oxalum iodide, comprising the steps of:

[0032] S1. Preparation of 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol: 19 parts by weight of cyclohexyl phenyl ketone, 15 parts of glycerin, 0.18 parts of Amberlyst-15 exchange resin, 0.12 Mix color-changing silica gel, heat up to 80°C, heat and stir for 90 minutes, filter, take the filtrate and add saturated sodium bicarbonate aqueous solution to wash, let the organic layer stand still, dry, and distill under reduced pressure to obtain material A; recrystallize material A with ethanol, Dry to obtain 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol;

[0033] S2. Preparation of 2-phenyl-2-cyclohexyl-4-piperidinylmethyl-1,3-dioxol: take 34 parts of piperidine in parts by weight, pass through argon, and add 52 parts obtained in S1 in sequence 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol, 1 part catalyst TiO 2 / Pt mix, adjust the temperature to 30°C, irradiate with a 400w high-pressure mercury lamp for 24 hours,...

Embodiment 2

[0036] A preparation method for oxalum iodide, comprising the steps of:

[0037]S1. Preparation of 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol: 21 parts by weight of cyclohexyl phenyl ketone, 13 parts of glycerin, 0.3 parts of Amberlyst-15 exchange resin, Mix evenly with 0.08 color-changing silica gel, heat up to 90°C, keep stirring for 60 minutes, filter, take the filtrate and add saturated sodium bicarbonate aqueous solution to wash, let the organic layer stand still, dry, and distill under reduced pressure to obtain material A; recrystallize material A with acetonitrile, Dry to obtain 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol;

[0038] S2. Preparation of 2-phenyl-2-cyclohexyl-4-piperidinylmethyl-1,3-dioxol: take 51 parts of piperidine in parts by weight, pass through argon, and add 26 parts obtained in S1 in sequence 2-phenyl-2-cyclohexyl-4-methanol-1,3-dioxol, 2 parts catalyst TiO 2 / Pt mix well, adjust the temperature to 10°C, irradiate with a 500w high-pressure mercu...

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Abstract

The invention discloses an oxapium iodide preparation method. The method comprises the steps of S1, preparing 2-phenyl-2-hexamethylene-4-methanol-1,3-dioxolane, S2, preparing 2-phenyl-2-hexamethylene-4-piperidinemethyl-1, 3-dioxolane, and S3, preparing the oxapium iodide. The step S1 comprises the steps of mixing uniformly cyclohexyl phenyl ketone, glycerol, Amberlyst-15 exchange resin and allochroic silicagel, heating, maintaining the temperature, stirring, filtering, taking the filtered solution, adding saturated sodium hydrogen carbonate aqueous solution for washing, keeping static, taking organic layer, drying, releasing pressure, distilling to acquire material A, purifying material A, drying to acquire 2-phenyl-2-hexamethylene-4-methanol-1, 3-dioxolane. The method has the advantages of being mild in reaction condition, simple in operation, suitable for industrialized production, low in material toxicity, easy and cheap for material access, low in cost and good in comprehensive yield rate.

Description

technical field [0001] The invention relates to the technical field of oxalum iodide synthesis, in particular to a preparation method of oxalum iodide. Background technique [0002] Oxalinium iodide is a kind of antispasmodic drug developed by Japanese Taisho Toyama Pharmaceutical Company, which was mentioned above in Japan in June 1984, and its trade name is This species is recorded in the Japanese Pharmacopoeia XIV edition. This product is mainly used clinically to treat pain caused by female genital spasm, gastrointestinal spasm, urethral spasm, biliary tract spasm, and dyskinesia. [0003] At present, there are no relevant literature reports about the preparation method of oxalamium iodide and its analogues in China. In foreign countries, only Japanese patents JP: 56-25175, JP: 56-30971 and JP: 56-71089 have been described, and their common characteristics are all based on 2-cyclohexyl-2-phenyl-4-p-toluenesulfonate Acyloxy-1,3-dioxolane is used as the starting materi...

Claims

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Application Information

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IPC IPC(8): C07D317/28
CPCC07D317/28
Inventor 王康林黄志生柏春雷张成栋
Owner HEFEI PINGGUANG PHARMA
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