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
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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. Moreove

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthetic method for drug intermediate diphenylethanedione
  • Synthetic method for drug intermediate diphenylethanedione
  • Synthetic method for drug intermediate diphenylethanedione

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1:

[0019] The method for synthesizing drug intermediate diphenyl ethylenedione includes the following steps:

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

[0021] B: Control the stirring speed to 150rpm, add 4mol of 30% isoamyl butyrate solution, add diocene dimethyl titanium in 5 times within 60min, continue the reaction for 2h, then add 1.2L with a mass fraction of 10% Sodium sulfate solution, stir for 90min, add 15% potassium carbonate solution to adjust the pH to 10, lower the temperature to 10℃, add 800ml 20% sodium chloride solution, precipitate solid, filter, the mass fraction is Wash 4 times with 40% didecylamine solution, wash 2 times with 60% p-cresol solution, recrystallize in 80% 3-dimethylaminopropionitr...

Example Embodiment

[0022] Example 2:

[0023] The method for synthesizing drug intermediate diphenyl ethylenedione includes the following steps:

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

[0025] B: Control the stirring speed to 180rpm, add 5mol of 32% isoamyl butyrate solution, add diocene dimethyl titanium in 6 times within 87min, continue the reaction for 2.2h, then add 1.2L with a mass fraction of 16 % Sodium sulfate solution, stir for 100min, add 17% potassium carbonate solution to adjust the pH to 10.5, lower the temperature to 12℃, add 800ml 22% sodium chloride solution, precipitate solids, filter, mass fraction Wash 5 times with 42% didecylamine solution, wash 3 times with 62% p-cresol solution, recrystallize in 83% 3-dimethylaminopropion...

Example Embodiment

[0026] Example 3:

[0027] The method for synthesizing drug intermediate diphenyl ethylenedione includes the following steps:

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

[0029] B: Control the stirring speed at 190rpm, add 6mol of 36% isoamyl butyrate solution, add diocene dimethyl titanium in 7 times within 90min, continue the reaction for 3h, then add 1.2L with a mass fraction of 17% Sodium sulfate solution, stir for 110min, add 22% potassium carbonate solution to adjust the pH to 11, reduce the temperature to 16℃, add 800ml of 26% sodium chloride solution, precipitate solids, filter, mass fraction Wash 6 times with 45% didecylamine solution, wash 4 times with 66% p-cresol solution, recrystallize in 87% 3-dimethylaminopropionitr...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C45/28C07C49/784
CPCC07C45/28C07C49/784
Inventor 关艮安
Owner CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products