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Production method of 1-H benzotriazole acetate

A technology of benzotriazole acetate and benzotriazole ethyl acetate, which is applied in the field of compound synthesis, can solve problems such as low yield and complicated process, and achieves convenient operation, simple production process and safety factor. high effect

Active Publication Date: 2014-08-20
NANTONG BOTAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The 1-H benzotriazole acetate produced by the above production method has good thermal stability and oil solubility, but the process is more complicated and the yield is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The production method of 1-H benzotriazole acetate:

[0018] Put a 250ml four-necked flask into a device with stirring, a thermometer, a condenser and a constant pressure dropping funnel, add 100ml of chloroform and 10ml of catalyst triethylamine in turn into the 250ml four-necked flask, start stirring, and slowly add 40ml After the absolute ethanol is fully dissolved, cool down with an ice bath, keep at 0°C, slowly add 30ml of chloroform solution containing 11.3g of 0.1mol chloroacetyl chloride dropwise, keep the reaction for 3 hours, filter to remove triethylamine hydrochloride, The filtrate was evaporated to dryness with a rotary evaporator, the solvent was recovered, and the residue was ethyl chloroacetate;

[0019] Put a 250ml four-necked flask in a device with stirring, a thermometer, a condenser and a constant pressure dropping funnel, add 100ml of absolute ethanol to the 250ml four-necked flask, start stirring, and add 11.9g of benzotriazole in batches , afte...

Embodiment 2

[0025] The production method of 1-H benzotriazole acetate:

[0026] Put a 250ml four-necked flask in a device with stirring, a thermometer, a condenser and a constant pressure dropping funnel, add 110ml of chloroform and 8ml of catalyst triethylamine in turn into the 250ml four-necked flask, start stirring, and slowly add 50ml After fully dissolving absolute ethanol, cool down with an ice bath, keep at 0°C, slowly add dropwise 30ml of chloroform solution containing 11.3g of chloroacetyl chloride, keep it warm for 3 hours, remove triethylamine hydrochloride by filtration, and spin the filtrate The evaporator is evaporated to dryness, and the solvent is recovered, and the residue is ethyl chloroacetate;

[0027] Put a 250ml four-necked flask in a device with stirring, a thermometer, a condenser and a constant pressure dropping funnel, add 120ml of absolute ethanol to the 250ml four-necked flask, start stirring, and add 11.9g of benzotriazole in batches After fully dissolving, a...

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Abstract

The invention discloses a production method of 1-H benzotriazole acetate. The method comprises the steps of synthesizing ethyl chloroacetate and synthesizing 1-H benzotriazole ethyl acetate; firstly adding trichloromethane and a catalyst namely triethylamine, dropping a trichloromethane solution containing chloroacetyl chloride, removing triethylamine hydrochloride by filtration, and evaporating filtrate to dryness by using a rotary evaporator, thereby obtaining a residue namely ethyl chloroacetate; adding absolute ethyl alcohol, benzotriazole and sodium hydroxide, filtering an ethanol solution containing ethyl chloroacetate to obtain a generated inorganic salt, concentrating the filtrate, precipitating crystals, and filtering to obtain a product. Compared with conventional production methods, the method disclosed by the invention can be used for greatly shortening the production time and greatly improving the production efficiency; 1-H benzotriazole acetate produced by using the method has good thermal stability and oil solubility, can be used for significantly improving the extreme pressure property of liquid paraffin under an appropriate additive amount and improving the bearing capacity of liquid paraffin, and can reach a yield of more than 90%.

Description

technical field [0001] The invention relates to a production method of 1-H benzotriazole acetate, which belongs to the field of compound synthesis. Background technique [0002] As people pay more and more attention to environmental issues, the development and research of green lubricating oil has gradually become a hot spot. According to the regulations of the German organization on lubricating oil additives, most of the existing additives used in mineral oil are not suitable for green lubricating oils, so the development and research of new additives is urgently needed. [0003] Studies have found that it has good tribological properties in mineral oil, and does not contain chlorine and metal elements in the molecule, and will not have adverse effects on the environment, but its solubility in base oil is poor. Benzotriazole has good tribological properties but poor solubility in mineral oil. In order to improve its solubility in mineral oil, three new lubricating oil add...

Claims

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Application Information

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IPC IPC(8): C07D249/18
CPCC07D249/18
Inventor 黄海波黄奎生王宏黄雪平
Owner NANTONG BOTAO CHEM
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