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Preparation method of 3-chloropropionyl chloride

A technology of chloropropionyl chloride and benzoyl chloride, applied in the preparation of acyl halides, organic chemistry, etc., can solve the problems of high risk, high production cost, and no technological value, and achieve the effect of simple process and low production cost

Active Publication Date: 2021-10-22
佳尔科生物科技南通有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010]1. The phosgene used in the direct method is highly toxic, and its production and use are strictly controlled by the state; and the production cost is high and the danger is great
[0011]2. The indirect method uses thionyl chloride as an acylating agent, which produces a large amount of sulfur dioxide, which will have a great impact on the environment, and it is difficult to recycle, and there is no process the value of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 72g of acrylic acid (1mol) and 0.01g of ferric chloride to a 500ml four-necked bottle equipped with a thermometer, condenser and drying tube, stir under nitrogen protection, add 225g of trichlorotoluene dropwise at 120°C, and complete the addition , after reacting for 5 hours, rectify under reduced pressure (vacuum degree 5mmHg, 5 theoretical plates, reflux ratio 1:3), collect 45-50 ℃ fraction 124g 3-chloropropionyl chloride respectively at the top of the tower [GC-MS, m / z (%): 136.5 (dissolved in absolute ethanol)], content 99.5%, yield 97.6%) and 70-75°C fraction 134g benzoyl chloride [GC-MS, m / z (%): 150 (dissolved in absolute ethanol)], content 99.1%, yield 95.4%.

Embodiment 2

[0032] Add 72g of acrylic acid (1mol) and 0.04g of ferric chloride to a 500ml four-necked bottle equipped with a thermometer, condenser and drying tube, stir under nitrogen protection, add 212g of trichlorotoluene dropwise at 60°C, and complete the addition After 12 hours of reaction, rectification under reduced pressure (vacuum degree 5mmHg, 5 theoretical plates, reflux ratio 1:3), respectively collect 123g of 3-chloropropionyl chloride at the top of the tower at 45-50 ° C [GC-MS, m / z (%): 136.5 (dissolved in absolute ethanol)], content 99.2%, yield 96.9% and 70-75°C fraction 135g benzoyl chloride [GC-MS, m / z (%): 150 ( Dissolved in absolute ethanol)], content 99.0%, yield 96.1%.

Embodiment 3

[0034] Add 72g of acrylic acid (1mol) and 0.02g of ferric chloride to a 500ml four-necked bottle equipped with a thermometer, condenser and drying tube, stir under nitrogen protection, add 199g of trichlorotoluene dropwise at 90°C, and complete the addition , after reacting for 8.5 hours, rectify under reduced pressure (vacuum degree 5mmHg, 5 theoretical plates, reflux ratio 1:3), collect 122g of 3-chloropropionyl chloride at the top of the tower respectively at 45-50 ° C [GC-MS, m / z (%): 136.5 (dissolved in absolute ethanol)], content over 99.1%, yield 96.1%) and 70-75°C fraction 134g benzoyl chloride [GC-MS, m / z (%): 150 (dissolved in absolute ethanol)], the content is over 99.3%, and the yield is 95.4%.

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PUM

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Abstract

The invention provides a preparation method of 3-chloropropionyl chloride, wherein the preparation method comprises the following steps: mixing acrylic acid with a certain amount of catalyst, dropwise adding a certain amount of trichlorotoluene at a certain temperature under the protection of nitrogen, reacting for a period of time, and performing vacuum rectification to respectively obtain 3-chloropropionyl chloride and benzoyl chloride. The preparation method has the following beneficial effects: 1) acrylic acid and trichlorotoluene are adopted as raw materials, 3-chloropropionyl chloride is prepared in the presence of a catalyst, and benzoyl chloride with wide application is produced as a byproduct; the reaction route is environment-friendly, the process is simple, no emission is generated, and the requirement of atom economy is met; and the technical problem that toxic raw materials are used in the prior art is solved, and the technical problem that by-products polluting the environment are possibly generated in the prior art is also solved; and 2) the method is low in production cost, and in addition, the reaction route is combined with the specific reaction conditions, so that the yield of the obtained product is quite high and reaches 95% or above.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of 3-chloropropionyl chloride. Background technique [0002] 3-Chloropropionyl chloride is an important intermediate of DuPont's new pesticide variety indoxacarb (commonly known as indoxacarb), and it is also an important pharmaceutical intermediate. Indoxacarb is a new type of sodium channel blocker developed by DuPont in 1992 and launched in 2001. It is also the first commercialized insecticide of this type. The agent blocks the sodium ion channel in the insect cells, disables the nerve cells, and prevents various pests of various crops through contact killing and stomach poisoning. Indoxacarb has a unique mechanism of action, and there is no cross-resistance with other insecticides. It is very safe for non-target insects, with low residues. It can be harvested 2 days after application, and can be used for integrated pest control and resistance m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C53/50C07C63/10
CPCC07C51/58C07C53/50C07C63/10
Inventor 王彩霞周革
Owner 佳尔科生物科技南通有限公司
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