Chemical synthetic method of 2-hydroxybenzimidazole

A technology for hydroxybenzimidazole and chemical synthesis, applied in the direction of organic chemistry, etc., can solve the problems of low conversion rate of 2-hydroxybenzimidazole and long synthesis time, and achieve the effects of high conversion rate and low energy consumption rate

Inactive Publication Date: 2018-04-20
中山市小榄企业服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of chemical synthesis method of 2-hydroxybenzimidazole, to solve the prior art proposed in the above-mentioned background technology, in the synthetic process of 2-hydroxybenzimidazole, can produce a large amount of harmful substances , and the conversion rate of 2-hydroxybenzimidazole is low, and the synthesis time is long

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  • Chemical synthetic method of 2-hydroxybenzimidazole

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Embodiment 1

[0020] see figure 1 , the present invention provides a kind of chemical synthesis method of 2-hydroxybenzimidazole, the synthetic raw material of described 2-hydroxybenzimidazole comprises: o-phenylenediamine, acid, catalyst and sodium hydroxide, and described 2-hydroxybenzimidazole The chemical synthesis method of imidazole comprises the steps:

[0021] S1: Mixing: Mix the acid and o-phenylenediamine, stir evenly, and then use a ball mill to fully ball mill;

[0022] S2: Heating: put the ball-milled powder in step S1 into a round-bottomed flask, add a catalyst, then heat in an oil bath to 120 degrees Celsius, stir and keep warm for 2 hours;

[0023] S3: heating up: raise the temperature to 160 degrees Celsius, and use microwave radiation to keep warm for 5 hours;

[0024] S4: Cooling: After the reaction is finished, cool, pour into distilled water, use sodium hydroxide solution to neutralize the precipitated solution until the pH is 8.2, filter with suction, wash, and dry t...

Embodiment 2

[0029] see figure 1 , the present invention provides a kind of chemical synthesis method of 2-hydroxybenzimidazole, the synthetic raw material of described 2-hydroxybenzimidazole comprises: o-phenylenediamine, acid, catalyst and sodium hydroxide, and described 2-hydroxybenzimidazole The chemical synthesis method of imidazole comprises the steps:

[0030] S1: Mixing: Mix the acid and o-phenylenediamine, stir evenly, and then use a ball mill to fully ball mill;

[0031] S2: Heating: put the ball-milled powder in step S1 into a round-bottomed flask, add a catalyst, then heat in an oil bath to 100 degrees Celsius, stir and keep warm for 1 hour;

[0032] S3: heating up: raise the temperature to 140 degrees Celsius, and use microwave radiation to keep warm for 3 hours;

[0033] S4: Cooling: After the reaction is completed, cool, pour into distilled water, use sodium hydroxide solution to neutralize the precipitated solution to a pH of 7.8, suction filter, wash, and dry to obtain a...

Embodiment 3

[0038] see figure 1 , the present invention provides a chemical synthesis method of 2-hydroxybenzimidazole, the synthetic raw materials of said 2-hydroxybenzimidazole include: o-phenylenediamine, acid, catalyst and sodium hydroxide, said 2-hydroxybenzimidazole The chemical synthesis method of imidazole comprises the steps:

[0039] S1: Mixing: Mix the acid and o-phenylenediamine, stir evenly, and then use a ball mill to fully ball mill;

[0040] S2: Heating: Put the ball-milled powder in step S1 into a round-bottomed flask, add a catalyst, then heat in an oil bath to 110 degrees Celsius, stir and keep warm for 1.5 hours;

[0041] S3: heating up: raise the temperature to 150 degrees Celsius, and use microwave radiation to keep warm for 4 hours;

[0042] S4: Cooling: After the reaction is finished, cool, pour into distilled water, use sodium hydroxide solution to neutralize the precipitated solution to a pH of 8, filter with suction, wash, and dry to obtain a crude product;

...

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Abstract

The invention belongs to the technical field of novel material, and more specifically relates to a chemical synthetic method of 2-hydroxybenzimidazole. The synthetic raw materials of 2-hydroxybenzimidazole comprise o-phenylenediamine, an acid, a catalyst, and sodium hydroxide. The chemical synthetic method comprises following steps: S1, mixing; S2, heating; S3, temperature increasing, wherein thetemperature is increased to 140 to 160 DEG C, microwave radiation is adopted, and the temperature is maintained for 3 to 5h; S4, cooling, wherein after reaction, an obtained product is cooled, distilled water is added, a sodium hydroxide solution is used for neutralizing of a precipitation solution until pH value ranges from 7.8 to 8.2; S5, crystallization, wherein a dried crude product is subjected to recrystallization with an ethanol aqueous solution for 2 to 4 times, and at last active carbon is adopted for decolouring. The chemical synthetic method is low in energy consumption rate, and high in 2-hydroxybenzimidazole conversion rate, no harmful substance is generated in synthetic process, energy saving and environment protection are realized.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a chemical synthesis method of 2-hydroxybenzimidazole. Background technique [0002] 2-Chlorobenzimidazole is a widely used intermediate in organic synthesis, widely used in the synthesis of medicines, pesticides, etc., especially as an intermediate in the synthesis of a series of antihistamines, for example, for the treatment of allergic conjunctivitis, urticaria The new anti-allergic drugs Mizolastin (mizolastine), Emedastine and so on. In the prior art, in the synthesis process of 2-hydroxybenzimidazole, a large amount of harmful substances will be produced, and the conversion rate of 2-hydroxybenzimidazole is low, and the synthesis time is long. Therefore, we propose a 2-hydroxybenzimidazole Chemical synthesis method of benzimidazole. Contents of the invention [0003] The object of the present invention is to provide a kind of chemical synthesis method of 2-hydroxy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D235/26
CPCC07D235/26
Inventor 梅锦初
Owner 中山市小榄企业服务有限公司
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