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Preparation method and application of tert-butyl acetylene

A tert-butylacetylene and reaction technology, which is applied in the preparation of amino-substituted functional groups, hydrocarbon production from halogen-containing organic compounds, organic chemistry, etc., can solve the problems of high price of bromobutyllithium, increased raw material cost, and reduced product purity, etc. To achieve the effect of providing purity, easier recovery, and improving conversion efficiency

Active Publication Date: 2022-07-22
湖北骐盛医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the synthesis process of tert-butylacetylene, bromobutyllithium is generally used as a catalyst, but bromobutyllithium is expensive and cannot be recovered, and its existence as an impurity will reduce the purity of the product and increase the cost of raw materials

Method used

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  • Preparation method and application of tert-butyl acetylene
  • Preparation method and application of tert-butyl acetylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The preparation method of a kind of tert-butylacetylene provided by this embodiment, comprises the following steps:

[0046] (1) add 400 kilograms of xylenes in the reactor, add 390 kilograms of phosphorus pentachloride in stages, stir to make it fully dissolved; 195 kilograms of pinacolone are added dropwise at 10 ° C, and the dropwise addition is completed in about 8 hours, and the reaction generates 2 ,2-dichloro-3,3-dimethylbutane;

[0047] After the completion of the reaction, add ice-water mixture to the reactor, stand for stratification; separate the organic layer, extract 270 kilograms of 2,2-dichloro-3,3-dimethylbutane, 2,2-dichloromethane The yield of -3,3-dimethylbutane was 93.1%;

[0048] (2) in dechlorination still, add 405 kilograms of potassium hydroxide, 180 kilograms of phosphoramide, 270 kilograms of 2,2-dichloro-3,3-dimethylbutane and 1000 kilograms of water, be warming up to 180 ℃ of reaction, and Control the reaction temperature not to exceed 250 ...

Embodiment 2

[0057] The preparation method of a kind of tert-butylacetylene provided by this embodiment, comprises the following steps:

[0058] (1) add 200 kilograms of xylenes in the reactor, add 180 kilograms of phosphorus pentachloride in stages, stir and make it fully dissolved; 180 kilograms of pinacolone are added dropwise at 30 ° C, and the dropwise addition is completed in about 7.5 hours, and the reaction generates 2 ,2-dichloro-3,3-dimethylbutane;

[0059] After the completion of the reaction, add ice-water mixture to the reactor, stand for stratification; separate the organic layer, extract 120 kilograms of 2,2-dichloro-3,3-dimethylbutane, 2,2-dichlorobutane The yield of -3,3-dimethylbutane was 89.6%;

[0060] (2) in dechlorination still, add 360 kilograms of sodium hydroxide, 100 kilograms of phosphoramide, 120 kilograms of 2,2-dichloro-3,3-dimethylbutane and 800 kilograms of water, be warming up to 180 DEG C of reaction, and Control the reaction temperature not to exceed 25...

Embodiment 3

[0068] The preparation method of a kind of tert-butylacetylene provided by this embodiment, comprises the following steps:

[0069] (1) in reactor, add 400 kilograms of xylene, add 130 kilograms of phosphorus pentachloride in stages, stir to make it fully dissolved; 300 kilograms of pinacolone are added dropwise at 25 ° C, and the dropwise addition is completed in about 13 hours, and the reaction generates 2 ,2-dichloro-3,3-dimethylbutane;

[0070] After the reaction is completed, add ice-water mixture to the reaction kettle, let stand for stratification; separate the organic layer, extract 92 kilograms of 2,2-dichloro-3,3-dimethylbutane, 2,2-dichlorobutane -3,3-dimethylbutane in 95% yield;

[0071] (2) in the dechlorination still, add 184 kilograms of sodium hydroxide, 70 kilograms of phosphoramide, 92 kilograms of 2,2-dichloro-3,3-dimethylbutane and 500 kilograms of water, be warming up to 180 ℃ of reaction, and Control the reaction temperature not to exceed 250 ℃, and the...

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Abstract

The invention discloses a preparation method and application of tert-butyl acetylene, and the preparation method comprises the following steps: dissolving phosphorus pentachloride in an organic solvent, dropwise adding pinacolone into the organic solvent at the temperature of lower than 30 DEG C, and reacting to generate 2, 2-dichloro-3, 3-dimethyl butane; the mass ratio of pinacolone to phosphorus pentachloride is (1-5): (1-2); after the reaction is finished, adding an ice-water mixture, standing for layering, separating an organic layer, and extracting 2, 2-dichloro-3, 3-dimethyl butane from the organic layer; the method comprises the following steps: mixing 2, 2-dichloro-3, 3-dimethyl butane, hydroxide and water, adding a phosphamide catalyst, heating to 160-250 DEG C, and reacting to generate tert-butyl acetylene; the mass ratio of the 2, 2-dichloro-3, 3-dimethyl butane to the hydroxide is 1: (3-6), and the mass ratio of the phosphamide to the 2, 2-dichloro-3, 3-dimethyl butane is 1: (1-1.5); extracting tert-butyl acetylene from the reaction liquid through atmospheric distillation; according to the method, the phosphamide is used as the catalyst, so that the reaction efficiency is improved, and the phosphamide has the characteristics of high boiling point and water miscibility, is easier to separate from the target product tert-butyl acetylene, and is beneficial to improving the purity of the product tert-butyl acetylene.

Description

technical field [0001] The present application relates to the technical field of pharmaceutical synthesis, and more particularly, to a preparation method and application of tert-butylacetylene. Background technique [0002] Terbinafine hydrochloride is an important pharmaceutical intermediate, which is mainly used in the synthesis of broad-spectrum antifungal drug terbinafine hydrochloride. Terbinafine hydrochloride is an allylamine drug that is effective against pathogenic fungi of the skin, hair, and nails including dermatophytes such as Trichophyton (eg, Trichophyton rubrum, Trichophyton mentagrophytes, Trichophyton verruca , Trichophyton officinalis, Trichophyton violaceum), Microsporum (such as Microsporum canis), Epidermophyton floccosum, and yeasts of the genera Candida (such as Candida albicans) and Pityrophytes have a wide range of Antifungal activity. And some studies have found that it has a unique effect in the treatment of fatty liver, and its market value and...

Claims

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Application Information

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IPC IPC(8): C07C1/30C07C11/22C07C209/08C07C211/30A61P31/10
CPCC07C1/30C07C17/18C07C209/08C07C17/16A61P31/10C07C2531/02C07C11/22C07C19/01C07C211/30C07C21/22Y02P20/584
Inventor 马友奇黄胜勇王超马玉露胡火炬
Owner 湖北骐盛医药科技有限公司
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