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A kind of synthetic method of iminostilbene

A technology of iminostilbene and a synthesis method, applied in directions such as organic chemistry, can solve problems such as high cost, inability to reuse water vapor, and achieve the effects of low cost, increased yield, and reduced production water

Active Publication Date: 2021-06-08
ZHEJIANG HUAZHOU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, in the process of preparing iminostilbene by the above method, a large amount of water vapor is consumed and cannot be reused, and the cost is relatively high.

Method used

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  • A kind of synthetic method of iminostilbene
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  • A kind of synthetic method of iminostilbene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A kind of synthetic method of iminostilbene is prepared from iminodibenzyl as starting material through dehydrogenation reaction, and its chemical reaction equation is as follows:

[0042]

[0043] Contains the following steps:

[0044] Step 1: Put iminodibenzyl into the melting tank and heat up to melt.

[0045] In step 2, the molten iminodibenzyl is transferred to a melting transfer tank, and then the molten iminodibenzyl is injected into a vaporization mixer through a metering pump and mixed with superheated steam into a catalytic bed for catalytic dehydrogenation.

[0046] Step 3, after the reaction is completed, enter the receiving tank, absorb with toluene, cool down, and separate layers to obtain an organic layer and a water layer, and take the water layer as a set of water for later use.

[0047] Step 4, take a certain amount of mantle water and mix with hydrochloric acid, pickle the organic layer, then take a certain amount of mantle water to wash the organ...

Embodiment 2

[0058] The method steps of this embodiment and the amount of materials used in each step are basically the same as those of Example 1. The difference is that this embodiment also includes step 6, where a certain amount of water is mixed with hydrochloric acid, and the refined mother liquor obtained in step 5 is Carry out pickling, and then take a certain amount of mantle water to wash the refined mother liquor, and the refined mother liquor can be used as an organic solvent in step 3 after being pickled and washed. The hydrochloric acid used for pickling in step 6 is 20 parts, and the used mantle water for pickling is 1000 parts; The mantle water used for washing in step 6 is 1000 parts. The hydrochloric acid used in step 6 is the hydrochloric acid of concentration 30%.

[0059] In this example, 439.5 g of iminostilbene was finally obtained, with a yield of 87.9% and a purity of 99.92% (GC).

Embodiment 3

[0061] The method steps of this embodiment and the amount of materials used in each step are basically the same as those of Embodiment 1, the difference being that the organic solvent used in Step 3 and Step 5 is replaced by xylene by toluene.

[0062] In this example, 429 g of iminostilbene was finally obtained, with a yield of 85.8% and a purity of 99.88% (GC).

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PUM

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Abstract

The present invention relates to the field of synthesizing pharmaceutical intermediates, more specifically, it relates to a method for synthesizing iminostilbene. The process requires the use of water vapor. When the product is recovered, the water vapor will be converted into liquid water, and the organic matter can be dissolved in the organic solvent used to recover the product to form an organic layer. The liquid water can be used as mantle water. It is used to pickle and wash the organic layer, reduce the consumption of production water and save the cost of the enterprise. After the organic layer is recrystallized and filtered, the crystallization of the product and refined mother liquor can be obtained. These refined mother liquors can be used as organic solvents to recover products, which can improve the utilization rate of organic solvents and increase the yield.

Description

technical field [0001] The invention relates to the field of synthesis of pharmaceutical intermediates, more specifically, it relates to a synthesis method of iminostilbene. Background technique [0002] Iminostilbene (IS), is an important pharmaceutical intermediate, commonly used in the synthesis of carbamazepine, oxcarbazepine, and can also be used to prevent and treat hepatitis C, as an anti-hemolytic drug, to synthesize rhodium catalyst ligands, and also to It is an important synthetic raw material in genetic engineering, materials science, etc., and its structural formula is as follows: [0003] [0004] The Chinese invention patent whose patent publication number is CN101307021B discloses a chemical synthesis method of iminostilbene, mainly using iminodibenzyl as the main raw material to synthesize, and its reaction equation is as follows: [0005] [0006] In this method, a sufficient amount of catalyst is filled on the fixed catalytic bed, and the temperature...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/22
CPCC07D223/22
Inventor 徐委岭王雷王坚坚
Owner ZHEJIANG HUAZHOU PHARMA CO LTD