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Synthetic method for drug intermediate diphenylethanedione

A technology of diphenylethanedione and a synthesis method is applied in the synthesis of pharmaceutical intermediate diphenylethylenedione, and the field of preparation of pharmaceutical intermediates, and can solve the health damage of reaction operators, high pollution treatment cost, and reaction process. Intense and other problems, to achieve the effect of reducing the risk factor of the reaction, reducing the production cost, and improving the reaction yield

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

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Problems solved by technology

However, this synthesis method will produce nitrous acid gas and cause pollution, which will cause harm to the health of the reaction operators. The reaction process is intense and the risk factor is high. Moreover, sodium cyanide itself is highly toxic and pollutes the environment. The cost of post-pollution treatment Higher, not conducive to reducing production costs, so it is necessary to propose a new synthetic method

Method used

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  • Synthetic method for drug intermediate diphenylethanedione
  • Synthetic method for drug intermediate diphenylethanedione
  • Synthetic method for drug intermediate diphenylethanedione

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The synthetic method of medicine intermediate diphenyl ketone, comprises the steps:

[0020] A: Add 2mol 2-bromo-2'-hydroxyl-diphenyl-2-methylethanone in the reaction vessel, raise the temperature to 50°C, then add 900ml of potassium chloride solution with a mass fraction of 9%, and react 2h, gradually increase the temperature, and increase the temperature to 70°C within 60min;

[0021] B: Control the stirring speed at 150rpm, add 4mol mass fraction of 30% isoamyl butyrate solution, add dicyclodimethyltitanium in 5 times within 60min, continue the reaction for 2h, then add 1.2L mass fraction of 10% sodium sulfate solution, stirred for 90min, adding a mass fraction of 15% potassium carbonate solution to adjust the pH to 10, lowering the temperature to 10°C, adding 800ml of a mass fraction of 20% sodium chloride solution to precipitate solids, filtering, the mass fraction was Wash 4 times with 40% didecylamine solution, wash 2 times with 60% p-cresol solution, recrystall...

Embodiment 2

[0023] The synthetic method of medicine intermediate diphenyl ketone, comprises the steps:

[0024] A: Add 2mol 2-bromo-2'-hydroxyl-diphenyl-2-methylethanone in the reaction vessel, raise the temperature to 58°C, then add 900ml of potassium chloride solution with a mass fraction of 12%, and react 2.1h, gradually increase the temperature, and increase the temperature to 75°C within 65min;

[0025] B: Control the stirring speed at 180rpm, add 5mol mass fraction of 32% isoamyl butyrate solution, add dicyclodimethyltitanium in 6 times within 87min, continue the reaction for 2.2h, then add 1.2L mass fraction of 16 % sodium sulfate solution, stirred for 100min, adding a mass fraction of 17% potassium carbonate solution to adjust the pH to 10.5, lowering the temperature to 12°C, adding 800ml of a mass fraction of 22% sodium chloride solution to precipitate solids, filtering, mass fraction Wash 5 times with 42% didecylamine solution, wash 3 times with 62% p-cresol solution in mass fr...

Embodiment 3

[0027] The synthetic method of medicine intermediate diphenyl ketone, comprises the steps:

[0028] A: Add 2mol 2-bromo-2'-hydroxyl-diphenyl-2-methylethanone in the reaction vessel, raise the temperature to 60°C, then add 900ml of potassium chloride solution with a mass fraction of 15%, and react 3h, gradually increase the temperature, and increase the temperature to 76°C within 80min;

[0029] B: Control the stirring speed at 190rpm, add 6 mol of isoamyl butyrate solution with a mass fraction of 36%, add dicyclodimethyltitanium in 7 times within 90 minutes, continue the reaction for 3 hours, and then add 1.2L with a mass fraction of 17% sodium sulfate solution, stirred for 110min, adding a mass fraction of 22% potassium carbonate solution to adjust the pH to 11, lowering the temperature to 16°C, adding 800ml of a mass fraction of 26% sodium chloride solution, precipitated solids, filtered, the mass fraction was Wash 6 times with 45% didecylamine solution, wash 4 times with 6...

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Abstract

The invention discloses a synthetic method for the drug intermediate diphenylethanedione. The synthetic method comprises the following steps: adding 2-bromo-2'-hydroxy-diphenyl-2-methylethanone into areaction vessel, raising a temperature, then adding a potassium chloride solution, carrying out a reaction, and gradually increasing the temperature; and controlling a stirring speed, adding an isoamyl butyrate solution, adding dimethyl titanocene in batches, continuing a reaction, then adding a sodium sulfate solution, carrying out stirring, adding a potassium carbonate solution to adjusting a pH value, lowering the temperature, adding a sodium chloride solution, allowing a solid to be precipitated, carrying out filtering, washing the solid with a didecylamine solution a plurality of times,then washing the solid with a cresol solution a plurality of times, carrying out recrystallization in a 3-dimethylaminopropionitrile solution, and then carrying out dehydration with a dehydrating agent to obtain the finished diphenylethanedione.

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 a pharmaceutical intermediate diphenylethylenedione. Background technique [0002] Diphenyl ketone is mainly used as pharmaceutical intermediates, photosensitizers for ultraviolet curing resins, pharmaceutical raw materials, organic synthesis intermediates and ultraviolet curing agents, and also used as insecticides. Most of the existing synthetic methods are obtained by condensing benzaldehyde and sodium cyanide to obtain benzoin, and then oxidizing it with nitric acid. However, this synthesis method will produce nitrous acid gas and cause pollution, which will cause harm to the health of the reaction operators. The reaction process is intense and the risk factor is high. Moreover, sodium cyanide itself is highly toxic and pollutes the environment. The cost of post-pollution trea...

Claims

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Application Information

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IPC IPC(8): C07C45/28C07C49/784
CPCC07C45/28C07C49/784
Inventor 关艮安
Owner CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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