Check patentability & draft patents in minutes with Patsnap Eureka AI!

Synthesis method of high-purity 4-chloro-4'-hydroxybenzophenone

A technology of hydroxybenzophenone and synthesis method, which is applied in the field of synthesis of high-purity 4-chloro-4'-hydroxybenzophenone, can solve the problems of rough reaction conditions, low purity, and many by-products, and achieve The effect of purification process is good, the temperature control is precise, and the effect of reducing by-products

Pending Publication Date: 2020-01-10
郎溪李仕化学品有限公司
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But we should formalize that the traditional synthetic route and the use of aluminum trichloride have many by-products and the overall purity is not high. The time control is not good, and the reaction conditions are relatively rough. In order to further optimize the traditional synthetic route, the present invention carries out detailed optimization work

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Synthetic process: (1) Put 735 parts of chlorobenzene and 150 parts of anisole into the reaction kettle and cool to below 5 degrees Celsius;

[0032] (2) Add a total of 120 parts of anhydrous aluminum trichloride in three batches, control the temperature below 5 degrees Celsius, and stir for 2 hours;

[0033] (3) Add dropwise a mixture of 245 parts of p-chlorobenzoyl chloride and 120 parts of chlorobenzene, control the reaction temperature at 0-5 degrees Celsius, and complete the addition within 10 hours;

[0034] (4) After adding, keep at 0-5 degrees Celsius and react for 1 hour;

[0035] (5) Heat up to room temperature, and then maintain 25 degrees Celsius for 1 hour;

[0036] (6) Add 150 parts of anhydrous aluminum trichloride at one time and stir for 0.5 hours;

[0037] (7) Heat up to 80 degrees Celsius, and react at constant temperature for 0.5 hours;

[0038] (8) Then raise the temperature to between 125 and 130 degrees Celsius, and react at constant temperatur...

Embodiment 2

[0046] Synthetic process: (1) Put 735 parts of chlorobenzene and 150 parts of anisole into the reaction kettle and cool to below 5 degrees Celsius;

[0047] (2) Add a total of 200 parts of anhydrous aluminum trichloride in three batches, control the temperature below 5 degrees Celsius, and stir for 4 hours;

[0048] (3) Add dropwise a mixture of 245 parts of p-chlorobenzoyl chloride and 120 parts of chlorobenzene, control the reaction temperature at 0-5 degrees Celsius, and complete the addition within 10 hours;

[0049] (4) After adding, keep at 0-5 degrees Celsius and react for 3 hours;

[0050] (5) Raise the temperature to normal temperature, and then maintain the reaction at room temperature for 3 hours;

[0051] (6) Add 150 parts of anhydrous aluminum trichloride at one time and stir for 2 hours;

[0052] (7) Heat up to 80 degrees Celsius, and react at constant temperature for 1 hour;

[0053] (8) Then heat up to 125-130 degrees Celsius, and react at constant temperatu...

Embodiment 3

[0061] Synthetic process: (1) Put 735 parts of chlorobenzene and 150 parts of anisole into the reaction kettle and cool to below 5 degrees Celsius;

[0062] (2) Put in a total of 160 parts of anhydrous aluminum trichloride in three batches, distribute each batch equally, control the temperature below 5 degrees Celsius, and stir for 3 hours;

[0063] (3) Add dropwise a mixture of 245 parts of p-chlorobenzoyl chloride and 120 parts of chlorobenzene, control the reaction temperature at 0-5 degrees Celsius, and complete the addition within 10 hours;

[0064](4) After adding, keep at 0-5 degrees Celsius and react for 2 hours;

[0065] (5) Raise the temperature to normal temperature, and then maintain the reaction at room temperature for 3 hours;

[0066] (6) Add 150 parts of anhydrous aluminum trichloride at one time and stir for 1 hour;

[0067] (7) Heat up to 80 degrees Celsius, and react at constant temperature for 0.5 hours;

[0068] (8) Then heat up to 125-130 degrees Celsi...

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 relates to a synthesis method of high-purity 4-chloro-4'-hydroxybenzophenone. The method comprises the following steps: cooling chlorobenzene and anisole to 5 DEG C or below; adding anhydrous aluminum trichloride in three batches, controlling the temperature, dropwise adding a mixed solution of p-chlorobenzoyl chloride and chlorobenzene, and controlling the reaction temperature; maintaining the low temperature after addition is finished, raising the temperature to normal temperature, and maintaining the normal temperature for a reaction; adding anhydrous aluminum trichloride at atime, and then carrying out a two-stage heating reaction; performing cooling hydrolysis; and performing centrifuging, washing the crude product with a sodium carbonate solution and a sodium hydroxidesolution, adjusting the pH value with hydrochloric acid, and centrifugally separating out the refined product. The fine temperature control is combined with the control of the reaction time to reducebyproducts, so the purity reaches 99.9% or above.

Description

technical field [0001] The present invention relates to a kind of synthetic method of medicine intermediate, especially a kind of synthetic method of high-purity 4-chloro-4'-hydroxybenzophenone. Background technique [0002] The purity of the drug, that is, the reduction and control of by-products, has a great impact on the efficacy and side effects of the drug. As the purity of pharmaceutical intermediates, the difference in purity of a few tenths of a percentage point will affect the sales and price of the product. [0003] 4-Chloro-4'-hydroxybenzophenone, referred to as 4-CBP, is an important intermediate of fenofibrate drugs. After its function was discovered, the research on its synthesis has not stopped. Although after years of development, a variety of catalysts and synthetic routes have emerged, but its classic traditional synthetic route still has a place in production. The fundamental reason is that aluminum trichloride is cheap and cheap, and the cost control is ...

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): C07C45/46C07C45/78C07C49/83
CPCC07C45/46C07C45/78C07C49/83
Inventor 李建平徐寿军吴卫清
Owner 郎溪李仕化学品有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com