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A kind of method for continuous synthesis of benzimidazole compounds

A technology for benzimidazole and compound, which is applied in the field of continuous synthesis of benzimidazole compounds, can solve the problems of low production efficiency, high discharge of three wastes, complicated production operation, etc., so as to reduce the generation of by-products, simplify the production process, reduce the The effect of production costs

Inactive Publication Date: 2018-05-22
上海鑫合医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the batch synthesis method has the advantages of simple method and convenient equipment, it also has disadvantages such as low production efficiency, high discharge of three wastes, and complicated production operations.

Method used

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  • A kind of method for continuous synthesis of benzimidazole compounds
  • A kind of method for continuous synthesis of benzimidazole compounds
  • A kind of method for continuous synthesis of benzimidazole compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] K / Al was first prepared by equal volume impregnation method 2 o 3 , to 10g specific surface area is 300m 2 g -1 , with an average pore diameter of 8nm and a pore volume of 0.8cm 3 / g, the particle size is 20 mesh Al 2 o 3 Add 8 mL of KNO containing 0.5 g K dropwise to the carrier 3 solution, impregnated for 8 hours, then dried at 100°C for 8 hours, and then fired at 400°C for 5 hours in an air atmosphere to obtain K / Al 2 o 3 . K / Al 2 o 3 Add 100mL of water, stir, adjust the temperature to 40°C, add 10mL of H 2 PdCl 4 solution (Pd content is 0.04g / mL) and 10mL Cu(NO 3 ) 2 Solution (Cu content is 0.05 g / mL), kept at 40°C for 5 hours, added KOH solution dropwise to adjust the pH value to 8, kept the solution temperature and stirred for 1.5 hours; filtered, and the filter cake was washed with deionized water until neutral; Vacuum drying at 110°C for 4h; then, calcining at 260°C for 4h, and finally reducing with hydrogen at 260°C for 4h to obtain Cu5wt%-Pd4wt%-...

Embodiment 2

[0042] Mg / Al was first prepared by equal volume impregnation method 2 o 3 , to 10g specific surface area is 250 m 2 g -1 , with an average pore diameter of 6nm and a pore volume of 0.7cm 3 / g, the particle size is 30 mesh Al 2 o 3 Add 7mL of Mg(NO 3 ) 2 solution, impregnated for 16h, then dried at 105°C for 10h, and then calcined at 450°C in an air atmosphere for 6h to obtain Mg / Al 2 o 3 . Mg / Al 2 o 3 Add 100mL of water, stir, adjust the temperature to 60°C, add 10mL of Pd(NO 3 ) 2 solution (Pd content is 0.05g / mL) and 10mL CuCl 2 solution (Cu content is 0.03g / mL), kept at 60°C for 3 hours, then added dropwise (NH 4 ) 2 CO 3 Adjust the pH value of the solution to 9, keep the solution temperature and stir for 2.5h; filter, wash the filter cake with deionized water until neutral; vacuum dry at 100°C for 5h; then, roast at 300°C for 6h, and finally at 300°C Reduction with hydrogen for 5h, that is, the corresponding loading of Cu3wt%-Pd5wt%-Mg2wt% / Al 2 o 3 catal...

Embodiment 3

[0044] Na / Al was first prepared by equal volume impregnation method 2 o 3 , to 10g specific surface area is 280 m 2 g -1 , with an average pore diameter of 12nm and a pore volume of 1.0cm 3 / g, the particle size is 40 mesh Al 2 o 3 Add dropwise 10mL of NaNO containing 0.4g Na to the carrier 3 solution, impregnated for 30 h, then dried at 110 °C for 12 h, and then calcined at 500 °C in an air atmosphere for 3 h to obtain Na / Al 2 o 3 . Na / Al 2 o 3 Add 100mL of water, stir, adjust the temperature to 70°C, add 10mL of Pd(C 2 h 3 o 2 ) 2 solution (Pd content is 0.02g / mL) and 10mL Cu(NO 3 ) 2 solution (Cu content is 0.07g / mL), kept at 70°C for 7 hours, added dropwise NaOH solution to adjust the pH value to 10, kept the solution temperature and stirred for 5 hours; filtered, and the filter cake was washed with deionized water until neutral; at 80 Vacuum drying at ℃ for 8h; then, roasting at 350℃ for 8h, and finally reducing with hydrogen at 350℃ for 5h, that is, to ob...

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Abstract

The invention discloses a method for continuously synthesizing a benzimidazole compound. The method comprises the steps:in a fixed bed reactor, firstly reducing and activating a loaded multi-metal solid catalyst by hydrogen; then using inert gas as carrier gas; adjusting the temperature to 130-250 DEG C and the pressure at 2-10 MPa; continuously introducing mixed raw materials of an ortho-nitroaniline compound shown in a formula (I), fatty alcohol shown in a formula (II) and distilled water iknto the fixed bed reactor by using a high pressure pump; feeding the reactants which are cooled by a condenser to a gas-liquid separator to collect a liquid product so as to obtain the benzimidazole compound shown in a formula (III), wherein the loaded multi-metal solid catalyst is a Cu-Pd-M / Al2O3 catalyst. According to the method disclosed by the invention, multiple intermittent reactions are changed to a one-step continuous reaction, so that the production process is simplified, generation of byproducts is reduced, the conversion rate can reach 100% to the maximum extent, and the yield of the target product benzimidazole compound can reach 99% to the maximum extent. The formulae are shown in the description.

Description

technical field [0001] The invention relates to a method for continuously synthesizing benzimidazole compounds from nitroaniline compounds and fatty alcohols under the action of a solid catalyst in a fixed-bed reaction. Background technique [0002] Benzimidazole compounds are an important class of organic intermediates. Because benzimidazole compounds have both benzene ring and imidazole ring, and the benzene ring and imidazole ring are on the same plane to form a more stable electron delocalization system, it has a special chemical structure. And electronic effects, it is its special structure and properties that determine the broad biological activity of benzimidazole compounds. This kind of compound has been widely used in the fields of medicine, pesticide, materials and the like. Therefore, the synthesis of benzimidazole compounds has aroused great interest, and great research progress has been made in recent years. [0003] The traditional synthesis methods of benzim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D235/08C07D235/06C07D235/18B01J23/89
CPCB01J23/8926B01J23/894B01J23/8946C07D235/06C07D235/08C07D235/18
Inventor 张群峰程正丰枫许孝良马磊卢春山李小年
Owner 上海鑫合医药有限公司
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