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Green production method of 1-(2, 3-dimethylphenyl)-1-chloroethane

A dimethylphenyl, green production technology, applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry and other directions, can solve problems such as unfavorable environmental protection and environmental pollution

Inactive Publication Date: 2020-03-27
南京恒道医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this method is also very significant, that is, the post-treatment of a large amount of hydrogen chloride gas introduced into the system during the reaction has brought great disadvantages to environmental protection, and if it is discharged directly, it will cause serious pollution to the environment

Method used

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  • Green production method of 1-(2, 3-dimethylphenyl)-1-chloroethane
  • Green production method of 1-(2, 3-dimethylphenyl)-1-chloroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The reaction product is qualitatively and quantitatively detected by high performance liquid chromatography: using octadecylsilane bonded silica gel as a filler (4.6mm×150mm, 5μm or a chromatographic column with equivalent performance), with 0.02mol / L disodium hydrogen phosphate solution (Adjust the pH value to 6.3 with phosphoric acid)-acetonitrile (75:25) as the mobile phase; the detection wavelength is 220nm, and the injection volume is 20 μl.

[0020] 1-(2,3-Dimethylphenyl)-1-ethanol and hydrogen chloride are passed into the 1-(2,3- In the reaction kettle of dimethylphenyl)-1-ethanol, heat it to the reaction temperature of 70°C, and vigorously stir the reaction for 5 hours. The hydrogen chloride produced in the reaction is extracted from the top of the reaction kettle and pumped into the bottom of the absorption tower. The flow rate is pumped into potassium hydroxide solution to absorb hydrogen chloride gas. The reaction solution was discharged from the bottom of t...

Embodiment 2

[0022] Reaction product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar proportion and each operating parameter are as follows:

[0023] 1-(2,3-Dimethylphenyl)-1-ethanol and hydrogen chloride are passed into the 1-(2,3- In the reaction kettle of dimethylphenyl)-1-ethanol, heat it to the reaction temperature of 50°C, and stir vigorously for 3 hours. The hydrogen chloride produced in the reaction is extracted from the top of the reaction kettle and pumped into the bottom of the absorption tower. The flow rate is pumped into the sodium hydroxide solution to absorb hydrogen chloride gas. The reaction solution was discharged from the bottom of the kettle, and after atmospheric distillation, high-purity 1-(2,3-dimethylphenyl)-1-chloroethane could be obtained with a yield of 87.6%.

Embodiment 3

[0025] Reaction product qualitative and quantitative detection method and operation are all the same as in Example 1, and the implementation steps of changing the reactant molar proportion and each operating parameter are as follows:

[0026] 1-(2,3-Dimethylphenyl)-1-ethanol and hydrogen chloride are passed into the 1-(2,3- In the reaction kettle of dimethylphenyl)-1-ethanol, heat it to the reaction temperature of 30°C, and vigorously stir the reaction for 1 hour. The hydrogen chloride produced in the reaction is extracted from the top of the reaction kettle and pumped into the bottom of the absorption tower. The flow rate is pumped into potassium carbonate solution to absorb hydrogen chloride gas. The reaction solution was released from the bottom of the kettle, and after atmospheric distillation, high-purity 1-(2,3-dimethylphenyl)-1-chloroethane could be obtained with a yield of 88.9%.

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Abstract

The invention relates to a green production method of 1-(2, 3-dimethylphenyl)-1-chloroethane. The method comprises the following steps of: introducing hydrogen chloride into a reaction kettle filled with 1-(2, 3-dimethylphenyl)-1-ethanol for reaction, feeding hydrogen chloride tail gas into the bottom of an absorption tower from the top of the reaction kettle, introducing an alkaline aqueous solution from the top of the absorption tower, absorbing hydrogen chloride gas, and discharging reaction liquid from the bottom of the reaction kettle to obtain 1-(2, 3-dimethylphenyl)-1-chloroethane. According to the process, hydrogen chloride generated in the production process of 1-(2, 3-dimethylphenyl)-1-chloroethane is effectively absorbed, so that the process is greener and more environment-friendly. The yield of the obtained reaction product 1-(2, 3-dimethylphenyl)-1-chloroethane is greater than 85%.

Description

technical field [0001] The invention belongs to the field of pharmacy, in particular to a method for producing 1-(2,3-dimethylphenyl)-1-chloroethane by using 1-(2,3-dimethylphenyl)-1-ethanol and hydrogen chloride The method relates to the preparation technology of 1-(2,3-dimethylphenyl)-1-chloroethane in the pharmaceutical field. Background technique [0002] Dexmedetomidine hydrochloride (dexmedetomidine hydrochloride) is the active dextrorotary form of medetomidine, which is a new type of α2-adrenoceptor agonist (sedative hypnotics) developed by Orion pharma / Abott. It has anti-sympathetic, Sedative and analgesic effects. The affinity for adrenergic receptors is 8 times higher than that of clonidine, the half-life is short, and the effective dose is small. It is suitable for sedation of patients who start intubation and use ventilators during intensive care treatment, and can improve hemodynamic stability and Reduce the incidence of myocardial ischemia. It was first laun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C22/04
CPCC07C17/16C07C22/04
Inventor 凌岫泉陶义华穆加兵
Owner 南京恒道医药科技股份有限公司
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