Chemical synthesis process for iminostilbene

An iminostilbene and chemical synthesis technology, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of many by-products, poor product quality, low product yield, etc., and achieve advanced process routes , low production cost and high reaction yield

Active Publication Date: 2008-11-19
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Before the present invention was made, in the chemical synthesis method of iminostilbene in the prior art, a kind of technique is to adopt the method preparation of bromination, dehydrobromination; Another kind of technique is to adopt the technology of catalytic dehydrogenation, as disclosed in EP570336 A kind of using iminodibenzyl as raw material, under the action of oxides containing Fe, K, Cr etc. catalytic dehydrogenation makes iminostilbene; EP0237952 discloses a kind of using iminodibenzyl as raw material, in Pt / C or Pd / C or Fe 2 o 3 Under catalysis, take o-nitrotoluene or dimethyl maleate as hydrogen acceptor, and react in xylene amine or xylene ether solvent to prepare iminostilbene; in these processes, the first process is due to the use of bromine As a bromination reagent, there are many by-products and low product yield; the catalyst used in the second process is generally more expensive, and the organic solvent used is more toxic or dangerous, and the product quality is poor.

Method used

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  • Chemical synthesis process for iminostilbene
  • Chemical synthesis process for iminostilbene
  • Chemical synthesis process for iminostilbene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The steam flow rate is 1.2L / h (calculated based on the volume of iminodibenzyl liquid, the flow rate is 0.1 times of the steam flow rate), and the fixed catalytic bed temperature is 520°C. The mass ratio of catalyst active components is: CaO: SiO 2 :ZnO:Gadolinium iron alloy (gadolinium content 75%)=1.5:1:1:0.5, active ingredient loading 40%.

[0019] In a Φ30×2-8 stainless steel tube with a height of 200cm, a Φ6×1 stainless steel coil is used for electric heating (power 2kw), and 1.0kg of catalyst is filled outside the inner coil of the stainless steel tube, and the temperature is controlled by a temperature control probe. The material goes through the shell. The two ends of the Φ30×2-8 stainless steel pipe are equipped with baffles to make the air flow evenly distributed, and a 10cm insulation layer is added.

[0020] The preparation process of the catalyst is as follows: mix zinc, silicon, calcium oxide and rare earth (gadolinium-iron alloy) in the silicone emulsio...

Embodiment 2

[0023] The steam flow rate is 1.2L / h, and the fixed catalytic bed temperature is 520°C. The mass ratio of catalyst active components is: CaO: SiO 2 : ZnO: gadolinium-iron alloy (gadolinium content 75%)=1:1:1:0.5, active ingredient loading 50%, catalyst dosage 1.0kg.

[0024] Other operations are the same as in Example 1, the product yield is 81.2%, and the purity is 96.3%.

Embodiment 3

[0026] The steam flow rate is 1.2L / h, and the fixed catalytic bed temperature is 520°C. The mass ratio of catalyst active components is: CaO: SiO 2 : ZnO: gadolinium iron alloy (gadolinium content 75%) = 1.5: 1: 1: 0.8, active ingredient loading 60%, catalyst dosage 1.0 kg.

[0027] Other operations are the same as in Example 1, the product yield is 86.3%, and the purity is 97.5%.

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Abstract

The invention provides a method for chemically synthesizing iminostilbene which is shown as a formula (I), comprising the following steps that: catalyst is filled on a fixed catalyst bed, the temperature of the catalyst bed is increased to between 400 and 600 DEG C by heating the catalyst bed electrically, iminodibenzyl which is shown as a formula (II) and is pre-heated to be liquated is sent to the fixed catalyst bed through high-pressure water vapour, the flow rate of the water vapour is controlled to between 0.2 and 20l/h by the iminodibenzyl fluid volume, and the material which passes through the fixed catalyst bed is put into a receiving device holding cooling water to produce the mixed fluid which is subject to moisture evaporation to dryness is crystallized again so that the iminostilbene is obtained. The method mainly has the advantages of high reaction yield coefficient up to 93.8 percent, low production, advanced process flow and convenient operation.

Description

(1) Technical field [0001] The invention relates to a chemical synthesis method of a pharmaceutical intermediate iminostilbene. (2) Background technology [0002] Iminostilbene is a key intermediate in the synthesis of carbamazepine. Carbamazepine is mainly used for the treatment of all types of epilepsy except absence seizures, the treatment of trigeminal neuralgia and the prevention of manic depression. [0003] Before the present invention was made, in the chemical synthesis method of iminostilbene in the prior art, a kind of technique is to adopt the method preparation of bromination, dehydrobromination; Another kind of technique is to adopt the technology of catalytic dehydrogenation, as disclosed in EP570336 A kind of iminodibenzyl is used as raw material, and iminostilbene is prepared by catalytic dehydrogenation under the action of oxides containing Fe, K, Cr, etc.; EP0237952 discloses a kind of iminodibenzyl as raw material, in Pt / C or Pd / C or Fe 2 o 3 Under ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/26B01J23/83
Inventor 苏为科梁现蕊蒋组林徐健康宋刚王其亮
Owner ZHEJIANG UNIV OF TECH
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