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Pipeline preparation method and device for 2-(4-bromomethylphenyl)propionic acid

A technology of bromomethylphenyl and methylphenyl, which is applied in the field of pipeline preparation of 2-propionic acid, can solve the problems of serious environmental protection and safety, increased process cost, and difficulty in separation and extraction, and achieves less three wastes and high atom utilization , good economic benefits

Active Publication Date: 2021-01-05
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the problem that exists in this operational route is the 3rd step bromination reaction, although this bromination reaction has all obtained higher yield, used sherwood oil as solvent in method 1, inflammable and explosive, dangerous Large, the solvent is banned for industrialization; in method 2, NBS is used as the brominated reagent and BPO is used as the initiator, which greatly increases the process cost. The key is that carbon tetrachloride is used as a solvent, which is highly toxic and is also a solvent that is banned for industrialization
[0027] In summary, the common problems of the above traditional synthesis methods are: expensive materials, complicated operation, many by-products, harsh conditions, difficult separation and extraction, serious environmental protection and safety

Method used

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  • Pipeline preparation method and device for 2-(4-bromomethylphenyl)propionic acid
  • Pipeline preparation method and device for 2-(4-bromomethylphenyl)propionic acid
  • Pipeline preparation method and device for 2-(4-bromomethylphenyl)propionic acid

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Experimental program
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Effect test

Embodiment 1

[0055] The structure of the reaction device is as figure 1 , the first tubular photoreactor with a built-in light source 9: the length of the vitreous pipe winding part is 10cm, the inner diameter is 10cm; the inner diameter of the jacket is 20cm; the length of the pipe is 1m, the diameter is 0.5mm, and the pipe material is polytetrafluoroethylene tube; the light source is a 250nm UV lamp with a diameter of 2mm. The second tubular photoreactor 10 with a built-in light source: the length of the winding part of the vitreous pipe is 20 cm, and the inner diameter is 10 cm; the inner diameter of the jacket is 20 cm; the length of the pipe is 30 m, the diameter is 1 mm, and the pipe material is a polytetrafluoroethylene pipe; The light source was a 250 nm UV lamp with a diameter of 2 mm.

[0056] The operation steps are as follows:

[0057] First turn on the light sources of the first tubular photoreactor 9 with a built-in light source and the second tubular photoreactor 10 with ...

Embodiment 2

[0059] The structure of the reaction device is as figure 1 , the first tubular photoreactor 9 with a built-in light source: the length of the winding part of the vitreous pipe is 25cm; the length of the pipe is 50m, and the diameter is 3mm; the light source is a 365nm UV lamp with a diameter of 2mm. The second tubular photoreactor 10 with a built-in light source: the length of the winding part of the vitreous tube is 25 cm; the length of the tube is 50 m, and the diameter is 2 mm; the light source is a 365nm UV lamp with a diameter of 2 mm. Others are the same as embodiment 1.

[0060] The first tubular photoreactor 9 preheating temperature with built-in light source is 60 ℃, and raw material 2-(4-methylphenyl) propionic acid and benzoyl peroxide (consumption is based on 2-(4-methylbenzene) The mass of base) propionic acid is 10%) dissolved in chloroform (solvent consumption is 8mL / g based on the mass of 2-(4-methylphenyl) propionic acid) and stored in the first reservoir 1,...

Embodiment 3

[0062] The structure of the reaction device is as figure 1 , the first tubular photoreactor 9 with a built-in light source: the length of the winding part of the vitreous pipe is 20cm; the length of the pipe is 30m, and the diameter is 1mm; the light source is a 365nm UV lamp with a diameter of 2mm. The second tubular photoreactor 10 with a built-in light source: the length of the winding part of the vitreous tube is 20 cm; the length of the tube is 30 m, and the diameter is 1 mm; the light source is a 365nm UV lamp with a diameter of 2 mm. Others are the same as embodiment 1.

[0063] The first tubular photoreactor 9 preheating temperature with built-in light source is 80 ℃, and raw material 2-(4-methylphenyl) propionic acid and benzoyl peroxide (consumption is based on 2-(4-methylbenzene) The mass of 2-(4-methylphenyl)propionic acid is 5%) dissolved in 1,2-dichloroethane (the amount of solvent is 6mL / g based on the mass of 2-(4-methylphenyl)propionic acid) and stored in No...

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Abstract

The invention discloses a pipelization preparation method and device for 2-(4-bromomethylphenyl)propionic acid and belongs to the technical field of pharmaceuticals. On one hand, the invention provides the pipelization preparation device for 2-(4-bromomethylphenyl)propionic acid, and the device comprises two tubular photoreactors internally provided with light sources, two mixers, three storage devices, three metering pumps, two water circulating pumps, two water bath kettles and one crystallization kettle. On the other hand, the invention provides the method for preparing 2-(4-bromomethylphenyl)propionic acid by using the device, and the method is simple in operation, mild in reaction condition, simple in aftertreatment, low in waste gas, waste water and waste residue production, high in atom utilization ratio, low in cost and high in economic benefit and is a green and environment-friendly process suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a method and a device for preparing 2-(4-bromomethylphenyl)propionic acid through pipelines. Background technique [0002] Loxoprofen sodium is an aryl propionic acid precursor non-steroidal anti-inflammatory drug developed by Japan Sankyo Co., Ltd. Its analgesic effect is remarkable, 10 to 20 times stronger than ketoprofen, indomethacin, and naproxen. Clinical experiments show that it is metabolized in the human body into trans -OH-type drugs, the concentration distribution in the liver and plasma is higher than other parts, and then quickly converted into glucose conjugates, and finally excreted in urine. [0003] 2-(4-Bromomethylphenyl)propionic acid is used as a key intermediate in the synthesis of loxoprofen sodium. There are many synthetic routes reported at home and abroad, and they are classified according to the preparation of different starting materials....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/58C07C51/363C07C51/43
CPCC07C51/363C07C51/43C07C57/58
Inventor 李坚军孙坚施阳裴金凤苏为科
Owner ZHEJIANG UNIV OF TECH
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