Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Synthesis method for 1-chloro-1-hydroxyl-4,4-diphenyl butyl-2-ketone

A technology of diphenylbutane and a synthesis method, which is applied in directions such as the preparation of heterocyclic compounds, organic chemistry, etc., can solve the problems of low total yield, difficult to scale up production, difficult to purify, etc., and achieve the effects of simple production and easy operation.

Inactive Publication Date: 2016-07-13
CHANGZHOU UNIV
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem mainly solved by the present invention: the synthesis route of 1-chloro-1-hydroxyl-4,4-diphenylbutan-2-one is long at present, the total yield is very low and less than 21%, and tert-butyl Lithium is relatively dangerous, not easy to scale up production, and difficult to purify. The invention provides a high yield and relatively safe synthesis of 1-chloro-1-hydroxyl-4,4-diphenylbutan-2-one method

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
  • Synthesis method for 1-chloro-1-hydroxyl-4,4-diphenyl butyl-2-ketone

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] Take 70mg of magnesium sulfate and put it into a 10mL flask with a stirring bar and a reflux device, then add 3mL of anhydrous ether to it, and then immediately install a Y-shaped feeding tube, and install a spherical tube with a drying tube on one end of the feeding tube. Condenser, the other port is covered with a rubber head, and then 450mg of chlorobenzene solution is injected from the rubber head into the flask using a 2mL syringe, and then the flask is moved to the electromagnetic stirring heater, and the rotation speed is set to Set at 180r / min, heat up until there is reflux liquid, reflux for 25min, filter while it is hot, collect the filtrate, put it in a three-necked flask, you can get phenylmagnesium chloride; weigh 230mg of 2-(2-methyl- 1,3-dioxolane-2-yl) ethyl acetate, its solution in 1mL of anhydrous ether, and then use a 2mL syringe to drop the mixed solution into the above-mentioned filtrate, after the dropwise addition is completed, the alkane Put the ...

example 2

[0019] Take 80mg of magnesium sulfate and put it into a 10mL flask with a stirring bar and a reflux device, add 4mL of anhydrous ether to it, and then immediately install a Y-shaped feeding tube, and install a spherical tube with a drying tube on one end of the feeding tube. Put a rubber head on the other end of the condenser tube, then inject 500mg of chlorobenzene solution from the rubber head into the flask using a 2mL syringe, then move the flask to the electromagnetic stirring heater, set the speed to Set at 200r / min, raise the temperature until there is reflux liquid, reflux for 30min, filter while it is hot, collect the filtrate, put it in a three-necked flask, you can get phenylmagnesium chloride; weigh 250mg of 2-(2-methyl- 1,3-dioxolane-2-yl) ethyl acetate, its solution in 2mL of anhydrous diethyl ether, and then use a 2mL syringe to drop the mixture into the filtrate obtained above, after the dropwise addition is completed, the alkane Put a reflux device on the bott...

example 3

[0021]Take 60mg of magnesium sulfate and put it into a 10mL flask with a stirring bar and a reflux device, add 2mL of anhydrous ether to it, and then immediately install a Y-shaped feeding tube, and install a spherical tube with a drying tube on one end of the feeding tube. Put a rubber head on the other end of the condenser tube, and then inject 400mg of chlorobenzene solution from the rubber head into the flask using a 2mL syringe, then move the flask to the electromagnetic stirring heater, and set the speed to Set at 150r / min, heat up until there is reflux liquid, reflux for 20min, filter while it is hot, collect the filtrate, put it in a three-necked flask, you can get phenylmagnesium chloride; weigh 220mg of 2-(2-methyl- 1,3-dioxolane-2-yl) ethyl acetate, its solution in 1mL of anhydrous ether, and then use a 2mL syringe to drop the mixed solution into the above-mentioned filtrate, after the dropwise addition is completed, the alkane Put a reflux device on the bottle and ...

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

PropertyMeasurementUnit
quality scoreaaaaaaaaaa
Login to View More

Abstract

The invention discloses a synthesis method for 1-chloro-1-hydroxyl-4,4-diphenyl butyl-2-ketone, and belongs to the field of organic synthesis techniques.For the defects that an existing synthetic route of 1-chloro-1-hydroxyl-4,4-diphenyl butyl-2-ketone is long, the total yield is very low and is no more than 21%, tert-butyllithium is used, danger exists, enlarged production is not easy to achieve, and extraction is not easy to achieve, the high-yield and safe synthesis method for 1-chloro-1-hydroxyl-4,4-diphenyl butyl-2-ketone is supplied.

Description

technical field [0001] The invention discloses a synthesis method of 1-chloro-1-hydroxyl-4,4-diphenylbutan-2-one, which belongs to the technical field of organic synthesis. Background technique [0002] β-amino ketones are key intermediates for the synthesis of β-amino alcohols, β-amino acids, β-lactams and other synthetic drugs or natural substances, and are widely used in organic synthesis. Studies have shown that β-aminoketone itself has various biological activities such as antibacterial, anti-inflammatory, anticancer, antiviral, sedative, and analgesic, and is an important class of biologically active substances. [0003] The synthesis route of 1-chloro-1-hydroxy-4,4-diphenylbutan-2-one is long, the total yield is very low, less than 21%, and tert-butyllithium is used, which is dangerous and not easy to scale up production. And not easy to purify. Contents of the invention [0004] The technical problem mainly solved by the present invention: the synthesis route of ...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/245C07C45/59
CPCC07C45/59
Inventor 陈兴权
Owner CHANGZHOU UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com