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Synthetic method for dicycloethyl piperidine drug intermediate benzophenone

A technology of bicycloethylpiperidine and benzophenone, which is applied in the preparation of pharmaceutical intermediates and the field of synthesis of bicycloethylpiperidine drug intermediate benzophenone, which can solve the adverse effects on the personal safety of synthesis operators, equipment manufacturing and Increased maintenance costs, high corrosion resistance requirements, etc., to achieve the effects of reducing pollution treatment costs, increasing reaction yield, and shortening reaction time

Inactive Publication Date: 2018-07-03
CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the benzyl chloride and benzene that this synthetic method adopts are carcinogens, have high toxicity, are unfavorable to the personal safety of synthetic operators, and the cost of pollution treatment in the later stage of the reaction is relatively high; High, equipment manufacturing and maintenance costs increase, these factors will lead to an increase in production costs, and the overall synthesis process of this method is relatively complicated, so it is necessary to propose a new synthesis method

Method used

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  • Synthetic method for dicycloethyl piperidine drug intermediate benzophenone
  • Synthetic method for dicycloethyl piperidine drug intermediate benzophenone
  • Synthetic method for dicycloethyl piperidine drug intermediate benzophenone

Examples

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Effect test

Embodiment 1

[0017] The synthetic method of benzophenone, a bicycline drug intermediate, comprises the steps:

[0018] A: Add 3mol benzhydryl ethyl ether into the reaction vessel, raise the temperature to 40°C, add 900ml of sodium sulfate solution with a mass fraction of 15% in 2 times within 60min, continue to stir, react for 2h, and then add 3mol tetrakis(triphenylphosphine)palladium powder, gradually increase the temperature, and rise to 55°C within 30min;

[0019] B: Then add 6 mol mass fraction of dimethyl fumarate solution with a mass fraction of 30%, control the stirring speed at 330rpm, continue the reaction for 90min, lower the temperature to 20°C, separate the layers of the solution, separate the oil layer, and the mass fraction is 10% Potassium chloride solution was washed 4 times, refluxed 3 times with 40% dibutylamine solution, 2 times with 50% diethylene glycol monobutyl ether solution, 70% 1,3- Recrystallize in dichloropropene solution and dehydrate with activated alumina d...

Embodiment 2

[0021] The synthetic method of benzophenone, a bicycline drug intermediate, comprises the steps:

[0022] A: Add 3mol benzhydryl ethyl ether to the reaction vessel, increase the temperature to 45°C, add 900ml of sodium sulfate solution with a mass fraction of 17% in 3 times within 75min, continue to stir, react for 2.5h, and then Add 3.5mol tetrakis(triphenylphosphine) palladium powder, gradually increase the temperature, and raise it to 57°C within 40min;

[0023] B: Then add 7mol mass fraction of dimethyl fumarate solution with a mass fraction of 33%, control the stirring speed at 345rpm, continue the reaction for 110min, lower the temperature to 22.5°C, separate the layers of the solution, separate the oil layer, and the mass fraction is 13% Potassium chloride solution was washed 5 times, refluxed 4 times with 42.5% dibutylamine solution, 3 times with 53% diethylene glycol monobutyl ether solution, 73% 1,3- Recrystallized in dichloropropene solution and dehydrated with anh...

Embodiment 3

[0025] The synthetic method of benzophenone, a bicycline drug intermediate, comprises the steps:

[0026] A: Add 3mol benzhydryl ethyl ether into the reaction vessel, raise the temperature to 47°C, add 900ml sodium sulfate solution with a mass fraction of 22% in 3 times within 90min, continue to stir, react for 3h, then add 4mol tetrakis(triphenylphosphine)palladium powder, gradually increase the temperature to 60°C within 50min;

[0027] B: Then add 8mol mass fraction of 37% dimethyl fumarate solution, control the stirring speed at 360rpm, continue the reaction for 130min, lower the temperature to 25°C, separate the layers of the solution, separate the oil layer, and the mass fraction is 16% Wash 5 times with potassium chloride solution, reflux 4 times with 45% dibutylamine solution, 3 times with 57% diethylene glycol monobutyl ether solution, 76% 1,3- Recrystallize in dichloropropene solution and dehydrate with activated alumina dehydrating agent to obtain 535.08 g of finis...

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Abstract

The invention discloses a synthetic method for the dicycloethyl piperidine drug intermediate benzophenone. The synthetic method is characterized by comprising the following steps: adding diphenylmethyl ethyl ether into a reaction vessel, raising a temperature, then adding a sodium sulfate solution in batches, continuing stirring and carrying out a reaction; then adding tetrakis(triphenylphosphine)palladium powder, gradually raising the temperature, then adding a dimethyl fumarate solution, controlling a stirring speed, and continuing the reaction; lowering the temperature, amd allowing the obtained solution to be layered so as to separate an oil layer; washing the oil layer with a potassium chloride solution a plurality of times, then carrying out refluxing with a dibutylamine solution a plurality of times, and then carrying out washing with a diethylene glycol monobutyl ether solution a plurality of times; carrying out recrystallization in a 1,3-dichloropropene solution and then carrying out dehydration with a dehydrating agent so as to obtain the finished benzophenone.

Description

technical field [0001] The invention relates to a method for preparing a pharmaceutical intermediate, which belongs to the field of organic synthesis, and in particular to a method for synthesizing benzophenone, a drug intermediate of bicycline. Background technique [0002] Benzophenone is an intermediate of ultraviolet absorbers, organic pigments, medicines, fragrances, and insecticides. In the pharmaceutical industry, it is used to produce dicyclohexyl piperidine, benzotropine hydrobromide, diphenhydramine hydrochloride, etc. The product itself is also a styrene polymerization inhibitor and a fragrance fixative. It can endow the fragrance with a sweet smell and is used in many perfumes and soap essences. Most of the existing synthetic methods are obtained by condensation of benzyl chloride and benzene, followed by oxidation with nitric acid. But the benzyl chloride and benzene that this synthetic method adopts are carcinogens, have high toxicity, are unfavorable to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/00C07C49/786
CPCC07C45/002C07C49/786
Inventor 关艮安
Owner CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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