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Synthetic method of alpha,alpha,alpha-trifluoro-p-tolualdehyde

A technology of trifluoromethylbenzaldehyde and its synthesis method, which is applied in the direction of chemical instruments and methods, preparation of carbonyl compounds by hydrolysis, organic compound/hydride/coordination complex catalyst, etc., and can solve the problems of harsh reaction conditions, difficult industrial production, Deal with problems such as high pressure to achieve catalyst stability, high reactivity and selectivity, and stable performance

Inactive Publication Date: 2019-01-01
阜新汉道化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Among them, the hydrolysis method of p-trifluoromethyldichloromethylbenzene is an existing mature production process. The hydrolysis process uses sulfuric acid with a high concentration for catalytic hydrolysis, so a large amount of waste acid will be produced, and the treatment pressure is relatively high.
And several other processing routes are difficult to realize industrialized production because of high cost or harsh reaction conditions

Method used

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  • Synthetic method of alpha,alpha,alpha-trifluoro-p-tolualdehyde
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  • Synthetic method of alpha,alpha,alpha-trifluoro-p-tolualdehyde

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preparation example Construction

[0044] The preparation condition of table 1 catalyst

[0045]

[0046]

[0047] The embodiment of the present invention uses gas chromatography to detect anisole, and the conditions are as follows:

[0048] GC Agilent 6890 equivalent instrument

[0049] FID detector, chromatography workstation

[0050] ZB-5 (30m×0.32mm×0.25μm) equivalent chromatographic column

[0051] Hydrogen flow rate: 30ml / min

[0052] Air flow rate: 300ml / min

[0053] Carrier gas (high purity nitrogen) flow rate: 1.0ml / min

[0054] Gasification chamber temperature: 260°C

[0055] Detector temperature: 260°C

[0056] Central control conditions:

[0057] Initial column temperature: 120°C

[0058] End column temperature: 260°C

[0059] Heating rate: 20°C / min

[0060] Product Conditions:

[0061] Column temperature: run at 100°C for 20min

Embodiment 1

[0062] The preparation of embodiment 1 p-trifluoromethylbenzaldehyde

[0063] ①Hydrolysis reaction: Put 250g (1mol) of industrial crude product p-trifluoromethyldichloromethylbenzene and catalyst No. 12.5g, stir and heat up to 110-120°C, at this temperature, slowly drop 50g deionized water into the reaction system through the dropping funnel, dropwise for 2.5h, after the dropwise addition, keep warm for 1h, take a sample from the kettle to test the three The remaining 0.14% of fluoromethyl dichloromethylbenzene (see the gas chromatogram for details figure 2 ), the reaction ends.

[0064] ②Post-treatment: ①After the reaction, the temperature of the kettle was lowered to 90°C, 10g of deionized water was added, and allowed to stand still for 1 hour, 55g of the water layer containing the catalyst was separated, and the organic phase was washed twice with 50g of deionized water to obtain the The crude product of tolualdehyde was 188g. After the washing water was combined with th...

Embodiment 2

[0066] The preparation of embodiment 2 p-trifluoromethylbenzaldehyde

[0067] The reaction process is the same as Example 1, and the difference from Example 1 is that in Example 1, No. 1 catalyst is replaced with No. 2 catalyst 25g, and 25g of deionized water is used. Others are unchanged, and 26g of catalyst is reclaimed after the reaction to obtain 99.2 % p-trifluoromethylbenzaldehyde 167g, the product yield is 95.1%, and the distillation residue is 2.9g.

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Abstract

The invention discloses a preparation method of alpha,alpha,alpha-trifluoro-p-tolualdehyde. Under the action of a self-made catalyst, alpha,alpha,alpha-trifluoro-p-benzyl bichloride and water generatea hydrolysis reaction, after the reaction is ended, reaction materials are washed and layered, the benzaldehyde product with 98.5% or above of gas phase content is obtained by purifying a benzaldehyde crude product, and the total product yield is up to 96% or above. The catalyst is recovered through vacuum drying of a water layer, and can be repeatedly used. Hydrogen chloride generated in the process is absorbed with water and can be prepared into hydrochloric acid. The method provided by the invention has excellent characteristics of simple process and environment protection such as less three wastes, thereby being more suitable for industrial mass production.

Description

technical field [0001] The invention relates to a preparation method of p-trifluoromethylbenzaldehyde, which belongs to the technical field of organic synthesis. Background technique [0002] p-Trifluoromethylbenzaldehyde is also known as 4-trifluoromethylbenzaldehyde, its English name is α, α, α-Trifluoro-p-tolualdehyde, its molecular formula is C8H5F3O, its relative molecular weight is 174.12, and it is a colorless liquid. As an important organic intermediate, it is widely used in pesticides, medicine and organic synthesis. In recent years, its use in the synthesis of new drugs has attracted much attention. Its synthetic route mainly contains: [0003] (1) p-trifluoromethyl dichloromethylbenzene hydrolysis method; [0004] (2) 1-(4-trifluoromethyl)phenyl-1-nitromethane oxidation method; [0005] (3) p-trifluoromethyl benzonitrile reduction method; [0006] (4) to trifluoromethyl benzoyl chloride hydrogenation method; [0007] (5) p-Trifluoromethylaniline diazonium sa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/55C07C45/43B01J31/02
CPCB01J31/0279B01J31/0284C07C45/43C07C47/55Y02P20/584
Inventor 侯光刘影刘军杨领军吴金江黄泽祎张晓宇于旭东陶金辉陈宝昌韩韬
Owner 阜新汉道化工有限责任公司
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