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Synthetic method for 1-chloro-3-methyl-3-buten-2-one

A synthesis method and technology of methyl isobutyl, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of heterocyclic compounds, etc., can solve the problems of difficult to scale up production, danger, and long synthesis route.

Inactive Publication Date: 2016-08-10
CHANGZHOU UNIV
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  • 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-3-methyl-3-buten-2-one is long at present, the total yield is very low and less than 32.5%, and the organic Solvent, relatively dangerous, not easy to enlarge production, and difficult to purify the problem, the present invention provides a kind of high yield, and the synthesis of 1-chloro-3-methyl-3-buten-2-one with short synthetic route method

Method used

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  • Synthetic method for 1-chloro-3-methyl-3-buten-2-one

Examples

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Comparison scheme
Effect test

example 1

[0017] Add 5mL of 1-(3-methyloxiranyl) ethyl ketone, 10mL of ether and 2mL of methyl isobutyl (methyl) ketone into a 50ml round bottom flask, mix well, and then use boron fluoride to dissolve the The air is exhausted, the flask is sealed, and after shaking by hand for 2 minutes, the gas in the flask is collected, and then 2 zeolites are added, and then a condenser tube is installed; the above-mentioned round bottom flask is heated and kept under reflux for 1 hour, then the heating is stopped, and the After the reactant was cooled to room temperature, the reflux device was changed to a distillation device, the receiving bottle was cooled with cold water, and heated to 114°C until the volume of the distillate was about 40% of the total volume of the reactant, and the effluent was collected to obtain 3 -Methyl-2,4-butanedione; add 10 mL of distilled water to the distillate obtained above using a dropping funnel, drop it within 3 minutes, and keep shaking, then transfer the mixture...

example 2

[0019] Add 10mL of 1-(3-methyloxiranyl) ethanone, 15mL of ether and 6mL of methyl isobutyl (methyl) ketone into a 50ml round bottom flask, mix well, and then use boron fluoride to dissolve the Vent the air, seal the flask, shake it by hand for 3 minutes, collect the gas in the flask, then add 2 zeolites, and then install a condenser tube; heat the above-mentioned round bottom flask, and keep it under reflux for 2 hours, then stop heating, wait for the After the reactant was cooled to room temperature, the reflux device was changed into a distillation device, the receiving bottle was cooled with cold water, and heated to 126°C until the volume of the distillate was about 60% of the total volume of the reactant, and the effluent was collected to obtain 3 -Methyl-2,4-butanedione; add 10 mL of distilled water to the distillate obtained above using a dropping funnel, drop it within 5 minutes, and keep shaking, then transfer the mixture into a beaker Pour 20mL of chlorine into it, s...

example 3

[0021] In a 50ml round bottom flask, add 10mL1-(3-methyloxiranyl)ethanone, 10mL ether and 4mL methylisobutyl (methyl)ketone, mix well, and then use boron fluoride to dissolve the The air is discharged, the flask is sealed, and after shaking by hand for 3 minutes, the gas in the flask is collected, and then 2 zeolites are added, and then a condenser is installed; the above-mentioned round bottom flask is heated and kept under reflux for 1 hour, then the heating is stopped, and the After the reactant was cooled to room temperature, the reflux device was changed to a distillation device, the receiving bottle was cooled with cold water, and heated to 118°C until the volume of the distillate was about 50% of the total volume of the reactant, and the effluent was collected to obtain 3 -Methyl-2,4-butanedione; add 10 mL of distilled water to the distillate obtained above using a dropping funnel, drop it within 5 minutes, and keep shaking, then transfer the mixture into a beaker Pour ...

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Abstract

The invention discloses a synthetic method for 1-chloro-3-methyl-3-buten-2-one, which belongs to the technical field of organic synthesis. The synthetic method of the invention has the advantages of high yield and short synthetic route and overcomes the problems of long synthetic route, low total yield of less than 32.5%, usage of hazardous organic solvents, great risks and difficulties in large-scale production and purification of traditional synthetic methods for 1-chloro-3-methyl-3-buten-2-one.

Description

technical field [0001] The invention discloses a synthesis method of 1-chloro-3-methyl-3-buten-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-3-methyl-3-buten-2-one is long, the total yield is very low, less than 32.5%, and a dangerous organic solvent 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 1-chloro-3-...

Claims

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Application Information

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IPC IPC(8): C07C49/227C07C45/66
CPCC07C45/66C07C45/58C07C45/64C07C49/227C07C49/173C07C49/185
Inventor 陈兴权
Owner CHANGZHOU UNIV
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