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4-n-butyl benzoyl chloride synthesis method

A technology of n-butylbenzoyl chloride and n-butylbenzoic acid, which is applied in the field of green synthesis of 4-n-butylbenzoyl chloride, can solve the problems of corrosion, high equipment requirements, high toxicity and the like, and achieves safe reaction operation. Simple, good application prospects, and the effect of less waste

Inactive Publication Date: 2018-07-20
江苏佳麦化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above method is simple to operate, but oxalyl chloride is a fuming liquid with a pungent odor, and it will decompose and generate toxic gases such as HCl and CO when it encounters moisture. Require
In addition, a small amount of highly toxic phosgene is produced in the by-products, which is highly corrosive after being exposed to moisture and will cause great damage to equipment.
Therefore, the safety of the production process is poor, the environmental hazards are great, and the requirements for equipment are high.

Method used

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  • 4-n-butyl benzoyl chloride synthesis method
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  • 4-n-butyl benzoyl chloride synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 300g of 4-n-butyltoluene, 0.9g of dibenzoyl peroxide, and 2 drops (about 0.15g) of triethanolamine into the reactor, close the reaction system, turn on the vacuum pump connected to the reaction system, and start to heat up to 95°C , then open the valve of the chlorine cylinder, and start to flow chlorine gas at a speed of 300ml / min. After 9h, the gas chromatography shows that the amount of 4-n-butyldichlorotoluene<0.05%, stop the flow of chlorine gas, and begin to drop to normal temperature, and the obtained chlorinated liquid 502 g was transferred to the drop tank.

[0028] Put 353.5g of 4-n-butylbenzoic acid into the reactor, raise the temperature to 120°C, and when it is completely melted, put 0.7g of ferric chloride into the reactor, stir evenly and start to add the chlorinated solution dropwise, and the dropwise addition is completed in 3 hours , After 8 hours of heat preservation, the gas chromatography showed that the amount of 4-n-butyltrichlorotoluene was <...

Embodiment 2

[0030] Put 300g of 4-n-butyltoluene, 0.9g of dibenzoyl peroxide, and 2 drops (about 0.15g) of triethanolamine into the reactor, close the reaction system, turn on the vacuum pump connected to the reaction system, and start to heat up to 70°C , then open the valve of the chlorine cylinder, and start to flow chlorine gas at a speed of 200ml / min. After 11 hours, gas chromatography shows that the amount of 4-n-butyldichlorotoluene<0.05%, stops the flow of chlorine gas, and starts to drop to normal temperature, and the obtained chlorinated liquid 500.5 g was transferred to the drop tank.

[0031] Put 357.5g of 4-n-butylbenzoic acid into the reactor, raise the temperature to 135°C, and when it is completely melted, put 1.2g of ferric chloride into the reactor, stir evenly and start to add the chlorinated solution dropwise, and the dropwise addition is completed within 3 hours , After 6 hours of heat preservation, the gas chromatography showed that the amount of 4-n-butyltrichlorotol...

Embodiment 3

[0033] Put 300g of 4-n-butyltoluene, 3g of dibenzoyl peroxide, and 3 drops (about 0.225g) of triethanolamine into the reactor, close the reaction system, turn on the vacuum pump connected to the reaction system, and start to heat up to 95°C. Then open the chlorine cylinder valve, start logical chlorine gas with the speed of 500ml / min, gas chromatography shows the amount<0.05% of 4-n-butyldichlorotoluene after 7h, stop logical chlorine gas, and begin to be down to normal temperature, gained chlorinated liquid 501.3 g Transfer to the drop tank.

[0034] Put 353g of 4-n-butylbenzoic acid into the reactor, raise the temperature to 145°C, and wait until it completely melts, put 1.75g ​​of ferric chloride into the reactor, stir evenly and start to add the chlorinated solution dropwise, and the dropwise addition is completed within 3 hours. After 5 hours of heat preservation, gas chromatography showed that the amount of 4-n-butyltrichlorotoluene was <0.05%, and the reaction was compl...

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Abstract

The invention discloses a 4-n-butyl benzoyl chloride synthesis method. The 4-n-butyl benzoyl chloride synthesis method comprises the following steps: (1) taking dibenzoyl peroxide as a catalyst and triethanolamine as an auxiliary catalyst, enabling 4-n-butyl methylbenzene and chlorine to have a chlorination to prepare a crude product of 4-n-butyl trichlorotoluene; and (2) enabling the crude product of 4-n-butyl trichlorotoluene and 4-n-butyl benzoic acid to have an acylation reaction with the participation of a catalyst ferric trichloride to prepare a target product 4-n-butyl benzoyl chloride.The fuming material oxalyl chloride is not needed, chlorine is introduced into the 4-n-butyl methylbenzene to generate 4-n-butyl trichlorotoluene, the 4-n-butyl trichlorotoluene and the 4-n-butyl benzoic acid are then reacted to generate the 4-n-butyl benzoyl chloride, the reaction operation is safe and simple, less three wastes are produced, no pollution to the environment is caused, the total yield of the product is more than 94%, the purity is more than 96%, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a green synthesis method of 4-n-butylbenzoyl chloride, which belongs to the technical field of fine chemical organic synthesis. Background technique [0002] 4-n-butylbenzoyl chloride is an important organic synthesis intermediate, molecular formula: C 11 h 13 ClO, CAS: [0003] 28788-62-7, the structural formula is as follows: [0004] [0005] 4-n-Butylbenzoyl chloride belongs to fine chemicals, is an important pharmaceutical intermediate and material intermediate, widely used in the synthesis of 4-butyl benzyl bromide, 4'-butyl acetophenone, 4-n- Butylbenzoic acid-4'-n-octyloxyphenyl ester, 4-butylbenzoic acid methyl ester, 1-n-butyl-4-[(4-n-butylphenyl)ethynyl]benzene and other important chemical Taste. [0006] The main method of industrially producing 4-n-butylbenzoyl chloride at present is that butylbenzene and excessive oxalyl chloride synthesize the target product under the participation of catalyzer aluminum t...

Claims

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Application Information

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IPC IPC(8): C07C17/14C07C22/04C07C22/06C07C51/60C07C63/10
CPCC07C17/14C07C51/60C07C22/04C07C22/06C07C63/10
Inventor 刘学峰徐松汪港郭维成
Owner 江苏佳麦化工有限公司