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Crude iminostilbene product recrystallization method

A technology of iminostilbene and recrystallization, applied in the direction of organic chemistry and the like, can solve the problems of low yield of iminostilbene synthesis process, low product purity, increased production cost, etc., and achieves high product purity, advanced process route and reaction. Yield improvement effect

Inactive Publication Date: 2016-05-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the current liquid-phase catalytic dehydrogenation to prepare iminostilbene, the crude product after removal of catalyst and solvent from the reaction liquid adopts a single solvent recrystallization process with low yield and low product purity, etc., the invention provides a mixed solvent recrystallization Process method
Compared with the existing single solvent recrystallization process, the mixed solvent recrystallization process can significantly increase the yield of iminostilbene finished products, save production costs, and solve the problems of increased production costs and low product purity caused by the low yield of iminostilbene synthesis process. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Add 10.0 g of iminostilbene crude product to a reactor with a heating, stirring and reflux device, then use a dropping device to drop a mixed solution of 320 mL of absolute ethanol and 10 mL of deionized water into the reactor, and start Stirring device, rotating speed is 250r / min, heat slowly to reflux state and maintain, stop heating after all solids are dissolved, add 10.0g powder decolorization activated carbon into the reactor after cooling slightly, heat to reflux and maintain for 20 minutes, then cool down and cool down, while hot The decolorized activated carbon was removed by filtration. The filtrate was left to cool and crystallize. After 24 hours, it was separated by suction filtration. The filter cake was washed three times with petroleum ether and dried to constant weight. Yield 94.0%, product purity 99.94% (GC).

Embodiment 2

[0019] Example 2: Add 10.0 g of iminostilbene crude product to a reactor with a heating, stirring and reflux device, then use a dropping device to drop a mixed solution of 420 mL of methanol and 10 mL of deionized water into the reactor, and turn on the stirring device , the rotation speed is 250r / min, slowly heated to the reflux state and maintained, stop heating after all the solids are dissolved, add 10.0g powdered decolorizing activated carbon to the reactor after cooling slightly, heat to reflux and maintain for 20 minutes, then cool down and filter while hot Decolorizing activated carbon. The filtrate was left to cool and crystallize. After 24 hours, it was separated by suction filtration. The filter cake was washed three times with petroleum ether and dried to constant weight. Yield 92.8%, product purity 99.92% (GC).

Embodiment 3

[0020] Example 3: Add 10.0 g of iminostilbene crude product to a reactor with a heating, stirring and reflux device, then use a dropping device to drop a mixed solution of 300 mL of isopropanol and 10 mL of deionized water into the reactor, and start stirring The device, with a rotating speed of 250r / min, slowly heated to reflux state and maintained, stopped heating after all the solids were dissolved, and added 10.0g powdered decolorizing activated carbon into the reactor after a little cooling, heated to reflux and maintained for 20 minutes, cooled down and filtered while hot Remove the decolorizing charcoal. The filtrate was left to cool and crystallize. After 24 hours, it was separated by suction filtration. The filter cake was washed three times with petroleum ether and dried to constant weight. Yield 94.2%, product purity 99.93% (GC).

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PUM

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Abstract

The invention discloses a crude iminostilbene product recrystallization method. The crude iminostilbene product recrystallization method comprises the steps that a crude iminostilbene product is added into a reactor with a heating, stirring and reflux device, then a certain proportion of a mixed solvent is added, electric heating is performed to reach a reflux state, stirring is maintained for a certain period of time, then cooling is performed, a certain mass ratio of decolorized activated carbon is added for decolorization, temperature rise is performed to reach the reflux state, the reflux state is kept for 20 minutes, the decolorized activated carbon is filtered and removed when being hot, and a crude iminostilbene producti is obtained through filtration after standing and crystallization. The crude iminostilbene product recrystallization method has the main advantages that compared with an existing single solvent crystallization process, a mixed solvent crystallization process is high in reaction efficiency (can be up to 94.2%), the product purity is high (can be up to 99.96%), recycle and reuse can be achieved after solvent rectification, a process route is advanced, the maneuverability is good, and the production costs are saved.

Description

technical field [0001] The invention belongs to the field of organic chemistry and relates to a method for recrystallization of crude iminostilbene. Specifically, the present invention relates to a method for recrystallizing the crude product of the reaction liquid prepared by liquid-phase catalytic dehydrogenation of iminostilbene after removal of catalyst and solvent from a mixed solvent to obtain iminostilbene finished product. Background technique [0002] Iminostilbene (IS), molecular formula: C 14 h 11 N, is an important pharmaceutical intermediate, commonly used in the synthesis of carbamazepine and oxcarbazepine, and can also be used in the prevention and treatment of hepatitis C, as an anti-hemolytic drug, in the synthesis of rhodium catalyst ligands, and also in genetic engineering, materials science important synthetic raw materials. [0003] At present, the domestic industrial method of producing iminostilbene is mainly the bromination method, using iminodiben...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/22
Inventor 张伟黄伟张蓉蓉杨怀青管庆宝王菡顾炜菁
Owner CHINA PETROLEUM & CHEM CORP
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