Preparation method of m-trifluoromethyl acetophenone oxime

A technology of trifluoromethyl acetophenone oxime and trifluoromethyl aniline is applied in the field of preparation of m-trifluoromethyl acetophenone oxime, and can solve the problem of high salt content in coupling liquid waste water, high three waste treatment costs, and high industrialization costs problems, to achieve the effect of reducing operating costs and equipment investment, reducing the cost of three wastes treatment, and high content and yield of finished products

Pending Publication Date: 2022-05-17
浙江欣禾生物股份有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Method (1) starting raw materials are expensive, and the cost of industrialization is relatively high; method (2) diazotization by-products obtains more sodium bisulfate, resulting in high salinity in the coupling liquid wastewater, which brings about a relatively high cost of industrial production of three wastes. High, and the post-processing of the coupling reaction is more complicated, resulting in about 65% of the finished product yield of m-trifluoromethyl acetophenone oxime, which is lower

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  • Preparation method of m-trifluoromethyl acetophenone oxime
  • Preparation method of m-trifluoromethyl acetophenone oxime

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Experimental program
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Effect test

Embodiment 1

[0029] Example 1: In step 2, dinitrogen solution was added dropwise, and the temperature was continued for 2 hours to obtain a coupling solution.

[0030] A kind of preparation method of m-trifluoromethyl acetophenone oxime, this preparation method comprises the steps:

[0031] Step 1: Under nitrogen protection, add 40% nitrosyl sulfuric acid (NOSO 4 H) 47.63g, start stirring and cool down to 5°C, slowly add m-trifluoromethylaniline 16.11g dropwise, continue to keep warm for 1h after the dropwise addition, then slowly add 161.10g water to dilute the diazonium solution, dropwise at 0°C, After the dropwise addition was completed, after decolorization and adsorption by activated carbon, a yellow clear diazonium salt solution was obtained by suction filtration, which was kept cold for later use.

[0032] Step 2: Under the protection of nitrogen, put 0.18mol of 50% acetaldehyde oxime solution, 40.28g of water and 0.008mol of copper sulfate catalyst in a 1000mL four-neck flask succ...

Embodiment 2

[0034] Embodiment 2: In step 2, the diazo solution is added dropwise, and the insulation is continued for 2.5h to obtain the coupling solution.

[0035] A kind of preparation method of m-trifluoromethyl acetophenone oxime, this preparation method comprises the steps:

[0036] Step 1: Under nitrogen protection, add 40% nitrosyl sulfuric acid (NOSO 4 H) 47.63g, start stirring and cool down to 7°C, slowly add m-trifluoromethylaniline 16.11g dropwise, continue to keep warm for 1.5h after the dropwise addition, then slowly add 161.10g water to dilute the diazonium solution, dropwise at 2°C After the dropwise addition was completed, after being decolorized and adsorbed by activated carbon, a yellow clear diazonium salt solution was obtained by suction filtration, which was kept cold for later use.

[0037] Step 2: Under the protection of nitrogen, put 0.18mol of 50% acetaldehyde oxime solution, 40.28g of water and 0.008mol of copper sulfate catalyst in a 1000mL four-neck flask succ...

Embodiment 3

[0039] Embodiment 3: In step 2, heavy nitrogen liquid is added dropwise, and the insulation is continued for 3h to obtain coupling liquid.

[0040] A kind of preparation method of m-trifluoromethyl acetophenone oxime, this preparation method comprises the steps:

[0041] Step 1: Under nitrogen protection, add 40% nitrosyl sulfuric acid (NOSO 4 H) 47.63g, start stirring and cool down to 8°C, slowly add m-trifluoromethylaniline 16.11g dropwise, continue to keep warm for 1.5h after the dropwise addition, then slowly add 161.10g water to dilute the diazonium solution, dropwise at 3°C After the dropwise addition was completed, after being decolorized and adsorbed by activated carbon, a yellow clear diazonium salt solution was obtained by suction filtration, which was kept cold for later use.

[0042] Step 2: Under the protection of nitrogen, put 0.18mol of 50% acetaldehyde oxime solution, 40.28g of water and 0.008mol of copper sulfate catalyst in a 1000mL four-neck flask successiv...

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Abstract

The invention discloses a preparation method of m-trifluoromethyl acetophenone oxime. On the premise of not adding an organic solvent, the diazo liquid prepared by diazotization of nitrosyl sulfuric acid and m-trifluoromethylaniline reacts with acetaldehyde oxime to obtain the m-trifluoromethylacetophenone oxime suspension, and the product with high content is directly extracted by a steam distillation method. According to the preparation method, the obtained product is high in content, the synthesis process is simple, easy to implement, economical and environmentally friendly, and the long-term strategic target of green and sustainable development is met.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of m-trifluoromethylacetophenone oxime. Background technique [0002] 3-Trifluoromethylacetophenone oxime, the English name is 3-Trifluoromethylacetophenone oxime, the molecular formula is C 9 h 8 f 3 NO, melting point 56~62℃, white needle-like crystal, is an important organic synthesis intermediate, mainly used in the fields of medicine, pesticide, dye and liquid crystal material. The preparation method reported in literature mainly contains following 2 kinds at present: (1) use dehydrated alcohol as solvent, adjust PH=8, after m-trifluoromethyl acetophenone and hydroxylamine hydrochloride reflux reaction insulation finishes, drop to room temperature, dropwise Adjust the pH to 2 with hydrochloric acid, precipitate crystals and obtain the finished product by suction filtration; (2) drop the sodium nitrite solution into the m-trifluoromethylanilin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/48C07C249/12C07C249/14
CPCC07C249/12C07C249/14C07C245/20C07C251/48
Inventor 顾建波潘胜节胡月赞徐惠兴李明吕述清丁露
Owner 浙江欣禾生物股份有限公司
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