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Synthetic technology of 3,5-dichloro-2-pentanone

A synthesis process and technology for mixtures, which are applied in the preparation of heterocyclic compounds, separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of reducing the reaction yield and increasing the difficulty of treatment of three wastes, etc., and achieve high purity and yield. The effect of chlorination reaction time and conversion rate improvement

Active Publication Date: 2017-01-04
HAIZHENG CHEM NANTONG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The target product synthesized by this type of method is easy to decompose under acidic and high temperature conditions, which reduces the reaction yield and increases the difficulty of three wastes treatment

Method used

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  • Synthetic technology of 3,5-dichloro-2-pentanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 4.8 Kg of glacial acetic acid (99.5%) and 21.3 Kg of concentrated hydrochloric acid (31%) in the 50 L reactor 4, start stirring and mix thoroughly and heat up to 70 o C; 12 Kg (purity 98%) α-chloro-α-acetyl-γ-butyrolactone and 292 g methyltrioctylammonium chloride are fully mixed in a mixer and then pumped into the premix liquid head tank 1 , the flow rate is controlled by the dropping flowmeter 2 to drop the premixed liquid into the reaction kettle; after the dropping, the temperature rises to 78-80 o C. After stirring for 30 minutes, turn on the vacuum to -0.08 MPa for steam distillation under reduced pressure, and keep the internal temperature at 78-80 o C, steam distilled for 2.5 hours until the distillate does not contain products; drop the balance pipe 3 to maintain the pressure balance in the premixed liquid head tank 1 and the reactor 4, so that the premixed liquid can flow smoothly into the reactor 4 Inside; the balance pipe 10 is used to maintain the pres...

Embodiment 2

[0027] Except that the acid added in the reactor was changed to 25.5 Kg concentrated hydrochloric acid (31%), all the others were the same as in Example 1. After the reaction was finished, 9.7 Kg of colorless 3,5-dichloro-2-pentanone was obtained with a purity of 94.8%. Yield 82.0%.

Embodiment 3

[0029] Except that the phase transfer catalyst was benzyltriethylammonium chloride, the others were the same as in Example 1. After the reaction, the purity of the final product 3,5-dichloro-2-pentanone was 95.2%, and the yield was 88.0%.

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Abstract

The invention relates to the field of a preparation technology of a fine chemical product, specifically to a synthetic technology of 3,5-dichloro-2-pentanone. The technology comprises the following steps: adding inorganic acid into a reaction vessel and stirring, heating to a certain temperature, adding alpha-chloro-alpha-acetyl-gamma-butyrolactone and a specific phase transfer catalyst into a mixer and fully mixing to prepare a premixed solution; pumping the premixed solution into a premixed solution elevated tank, metering by a stactometer and dropwise adding the solution into the above reaction vessel; carrying out thermal insulation and stirring for a certain period of time after dropwise addition, beginning reduced steam distillation, condensing a distillate in the reaction vessel by a condenser, letting the condensed distillate enter a laminator and layering, letting a water layer automatically flow back into the reaction vessel through a water-layer return pipe, and putting a product into a product storage tank through a product exit tube. By the synthetic technology of 3,5-dichloro-2-pentanone, the purposes of reaction safety, short reaction time, high yield and easy industrialization are achieved.

Description

technical field [0001] The invention relates to the technical field of preparation of fine chemical products, in particular to a synthesis process of 3,5-dichloro-2-pentanone. [0002] technical background [0003] Prothioconazole is a new broad-spectrum triazolethione fungicide developed by Bayer, patent number: WO9616048, application date: November 8, 1995, not only has good systemic activity, but also has excellent protection and treatment and eradication activity, and long-lasting. Since 2004, it has been registered in many countries, occupying the third place in Bayer's top 10 product list, and its sales in 2013 reached 750 million US dollars. 3,5-dichloro-2-pentanone is not only an important intermediate in the synthesis of prothioconazole, but also used in the synthesis of drugs for the treatment of senile insomnia and delirium tremens: clomethiazole hydrochloride; it can also be used for synthesis inhibition Leukemia and anti-tumor medicinal compounds: 3-(2-chloroet...

Claims

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Application Information

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IPC IPC(8): C07C45/59C07C45/84C07C49/16
CPCC07C45/59C07C45/84C07C49/16
Inventor 王建忠王丽敏包如胜罗红波蒋富国徐坚勇
Owner HAIZHENG CHEM NANTONG CO LTD
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