Preparation method of cyclopropyl acetylene important intermediate cyclopropylmethyl ketone

A technology of cyclopropyl methyl ketone and cyclopropyl acetylene is applied in the field of preparation of cyclopropyl methyl ketone, an important intermediate of cyclopropyl acetylene, and can solve the problems of low yield, difficult to obtain raw materials, high cost of raw materials, etc. The effect of improving reaction selectivity and conversion rate, improving space-time yield and selectivity, and improving reaction conversion rate

Active Publication Date: 2013-08-07
JIANGSU YUXIANG CHEM
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0010] In addition, there are synthetic methods using cyclopropylethanol as raw materials and synthetic methods using cyclopropylnitroethane as raw materials, which are expensive and have no industrial value.
[0011] In summary, there are various defects in the existing synthetic method...

Method used

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  • Preparation method of cyclopropyl acetylene important intermediate cyclopropylmethyl ketone

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Effect test

Embodiment 1

[0027] See the attached figure: After the preheated 5-chloro-2-pentanone and alkaline aqueous solution (5) enter the tower from the middle of the tower, they pass through the reaction separation section (6) and the reaction section (4), and a ring closure reaction occurs to form a ring Propyl methyl ketone. Since the generated cyclopropylmethyl ketone has a boiling point (110°C) lower than that of 5-chloro-2-pentanone, it is distilled out of the reaction section (4), so that the balance of the cyclization reaction shifts towards the generation of cyclopropylmethyl The direction of the ketone moves. As the reaction proceeds, the cyclopropyl methyl ketone is continuously distilled off, then passes through the separation section (3), and is collected from the top 2 of the tower to obtain the cyclopropyl methyl ketone product. The raw materials that have not been completely converted through the reaction section are separated by the reaction separation section (6), and then heate...

Embodiment 2

[0031] In a tower reactor with a length of 1m, the separation section (3) and the reaction section (4) are filled with 40g of glass spring rectification tower packing respectively, and the reaction separation section (6) is filled with 25g of glass spring rectification tower packing. 5-Chloro-2-pentanone and 30% KOH solution are mixed in a 1:2 mol ratio and then fed at a certain flow rate in the middle of the tower, staying at 150°C for 1 hr, and can be collected at the top of the tower to obtain cyclopropyl methyl ketone , content 99.2%, yield 95.6%.

[0032]

Embodiment 3

[0034] In a tower reactor with a length of 1m, the separation section (3) and the reaction section (4) are filled with 40g of glass spring rectification tower packing respectively, and the reaction separation section (6) is filled with 25g of glass spring rectification tower packing. 5-Chloro-2-pentanone and 30% NaOH solution are mixed in a 1:1 mol ratio and then fed at a certain flow rate in the middle of the tower, staying at 90°C for 2 hours, and can be collected at the top of the tower to obtain cyclopropyl methyl ketone , content 99.4%, yield 96.5%.

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Abstract

The invention relates to a preparation method of a cyclopropyl acetylene important intermediate cyclopropylmethyl ketone. The invention adopts a technical scheme that: 5-chloro-2-pentanone is adopted as an initial raw material; under an alkaline condition and in a multistage reactor, a reaction is carried out with a reactive distillation technology, wherein a reaction temperature is controlled at 90-150 DEG C; and cyclopropylmethyl ketone is obtained in the multistage reactor. According to the invention, the reaction is carried out with the reactive distillation technology. Reaction and distillation are carried out simultaneously, such that the reaction process is simplified. Therefore, the operation is simple, and reaction can be continuously carried out. A cyclization reaction is carried out in the multistage reactor, such that space-time yield and selectivity of the reaction are improved. The reaction is carried out with the reactive distillation technology, such that reaction product is continuously removed, and reaction conversion rate is greatly improved. Because reaction selectivity and conversion rate are improved, three-waste production is greatly reduced, original steps of stratification and extraction are eliminated, and cost is reduced. The method is a green synthesizing process.

Description

technical field [0001] The invention relates to a preparation method of cyclopropylmethyl ketone, an important intermediate of cyclopropyne. Background technique [0002] Cyclopropyl methyl ketone, the English name of Cyclopropyl methyl ketone, is a yellow or slightly yellow transparent liquid with a certain solubility in water and can be miscible with alcohol ethers. The molecular formula is as follows [0003] . [0004] [0005] Cyclopropyl methyl ketone is an important intermediate in the synthesis of cyclopropyne, which is an important intermediate in the anti-AIDS drug efavirenz. Cyclopropylmethyl ketone is an indispensable drug intermediate for the synthesis of such drugs, and is of great significance for the synthesis of cyclopropyne. [0006] Synthetic methods of cyclopropyl methyl ketone are generally divided into the following categories: [0007] 1. CN1994996 reports a preparation method of cyclopropyl methyl ketone. Add acetyl n-propanol to hydrochloric ...

Claims

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Application Information

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IPC IPC(8): C07C49/293C07C45/61B01D3/14
CPCY02P20/10
Inventor 黄小庭张治国程云涛李清龙程红伟
Owner JIANGSU YUXIANG CHEM
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