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Preparation method for N-2-methylphenylhydroxyamine

A technology of o-methylphenylhydroxylamine and o-nitrotoluene is applied in the field of preparation of o-methylphenylhydroxylamine, and can solve the problems of complex hydrogenation reduction reaction process, low product content and yield, and increased three-waste treatment costs, etc. , to achieve the effect of low cost, high recovery rate, and non-toxic recovery rate

Inactive Publication Date: 2016-12-07
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current preparation method of hydroxylamine has the following problems: 1) the catalyst used in the present invention is expensive, easily deactivated and difficult to regenerate and recycle; In addition to hydroxylamine, there are many by-products, resulting in low product content and yield, and poor product purity; 3) The waste water and waste residue produced by the method of the present invention are serious, which greatly increases the three wastes treatment cost of the enterprise

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Embodiment 1: a kind of preparation method of o-methylphenyl hydroxylamine, concrete preparation steps are:

[0011] (1) Preparation of catalyst: take 0.004g of NiCl 2 Loaded to 0.996g γ-Al by impregnation method 2 o 3 on, then calcined and reduced to prepare nano-nickel / γ-Al 2 o 3 Catalyst, named Catalyst A.

[0012] (2) Add 100g of o-nitrotoluene, 400g of solvent and 0.1g of catalyst A into a four-necked flask, then raise the temperature and add hydrazine hydrate dropwise. After the addition, stir and react at a temperature of 45°C for 2h, and take samples for central control. After the control is qualified, the reaction ends; filter while hot, wash the filter cake with absolute ethanol, concentrate under reduced pressure, then add water to precipitate a solid, filter and dry to obtain the product. The product yield reaches 98.5%, and the product content is 99.2%.

Embodiment 2

[0013] Embodiment 2: a kind of preparation method of o-methylphenyl hydroxylamine, concrete preparation steps are:

[0014] (1) Preparation of catalyst: Take 0.004g of NiCl 2 Loaded to 0.996g γ-Al by impregnation method 2 o 3 on, then calcined and reduced to prepare nano-nickel / γ-Al 2 o 3 Catalyst, named Catalyst A.

[0015] (2) Add 100g of o-nitrotoluene, 400g of solvent and 0.05g of catalyst A into a four-necked flask, then raise the temperature and add hydrazine hydrate dropwise. After the control is qualified, the reaction ends; filter while hot, wash the filter cake with absolute ethanol, concentrate under reduced pressure, then add water to precipitate a solid, filter and dry to obtain the product. The product yield reaches 99%, and the product content is 99.6%.

Embodiment 3

[0016] Embodiment 3: a kind of preparation method of o-methylphenyl hydroxylamine, concrete preparation steps are:

[0017] (1) Preparation of catalyst: Take 0.004g of NiCl 2 Loaded to 0.996g γ-Al by impregnation method 2 o 3 on, then calcined and reduced to prepare nano-nickel / γ-Al 2 o 3 Catalyst, named Catalyst A.

[0018] (2) Add 100g o-nitrotoluene, 300g solvent and 0.05g catalyst A into a four-neck flask, then raise the temperature and add hydrazine hydrate dropwise. After the control is qualified, the reaction ends; filter while hot, wash the filter cake with absolute ethanol, concentrate under reduced pressure, then add water to precipitate a solid, filter and dry to obtain the product. The product yield reaches 98.3%, and the product content is 99.0%.

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Abstract

The invention discloses a preparation method for N-2-methylphenylhydroxyamine, and belongs to the technical field of compound synthesis. According to the preparation method, the N-2-methylphenylhydroxyamine is synthesized by taking ortho-nitrotoluene as a raw material, taking hydrazine hydrate as a reducing agent, and taking a nano-nickel / gamma-Al2O3 material as a catalyst; the reaction yield can reach 98.0 percent or higher, and by-products are equal to or lower than 0.1 percent. The nano-nickel / gamma-Al2O3 material adopted by the preparation method has extremely strong reducing property; the catalytic activity and the selectivity are much higher than those of a conventional raney nickel catalyst; moreover, the catalyst is environment-friendly, short in reaction period, high in product quality and high in yield, can be applied repeatedly, reduces the emission of waste gas, waste water and waste residues, meets the requirement on green chemical process, and has a very industrial application value.

Description

Technical field: [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a preparation method of o-methylphenylhydroxylamine. Background technique: [0002] Pyraclostrobin, also known as pyraclostrobin, is a broad-spectrum methyl methoxyacrylate fungicide with a pyrazole structure discovered by BASF in 1993. The synthetic route of pyraclostrobin reported in the current literature is to use o-nitrotoluene as a raw material through reduction to o-methylphenylhydroxylamine, and then react with methyl chloroformate and dimethyl sulfate. The raw materials are easy to get. It is easy for industrial production, so the preparation of o-methylphenylhydroxylamine becomes the key. [0003] The current preparation method of hydroxylamine has the following problems: 1) the catalyst used in the present invention is expensive, easily deactivated and difficult to regenerate and recycle; In addition to hydroxylamine, there are many by-product...

Claims

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Application Information

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IPC IPC(8): C07C239/10B01J23/755
CPCC07C239/10B01J23/755
Inventor 韦琛鸿刘敏胡玉兵唐先龙吴海峡陈后福
Owner ANHUI COSTAR BIOCHEM CO LTD
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