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Novel pymetrozine intermediate nicotinaldehyde synthesis method and synthesis device

A synthetic method, the technology of pymetrozine, which is applied in the field of synthetic process of pesticide intermediates, can solve the problem that the synthetic process of nicotinic aldehyde cannot be applied to large-scale production, etc., and achieve the effect of simple process steps

Active Publication Date: 2021-03-30
JIANGSU ANPON ELECTROCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problem that the existing nicotine aldehyde synthesis process cannot be applied to large-scale production, the present invention proposes a new pymetrozine intermediate nicotine aldehyde synthesis method and synthesis device

Method used

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  • Novel pymetrozine intermediate nicotinaldehyde synthesis method and synthesis device
  • Novel pymetrozine intermediate nicotinaldehyde synthesis method and synthesis device
  • Novel pymetrozine intermediate nicotinaldehyde synthesis method and synthesis device

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preparation example Construction

[0026] A new method for synthesizing pymetrozine intermediate nicotinaldehyde, comprising the steps of:

[0027] S101: dissolving 3-picoline in 10-50% acetic acid solution to prepare a mixed solution;

[0028] S102: adding 1-10% by mass fraction of the main catalyst and 1%-50% by mass fraction of the co-catalyst to the mixed solution;

[0029] S103: airtightly fill with oxygen and react under predetermined conditions. After cooling to room temperature, distill off acetic acid under reduced pressure, add water and ester solvent to dissolve the residue and filter.

[0030] Further, the main catalyst is a nitrogen hydroxyl compound, including compound I, compound II and compound III.

[0031] Further, the molecular formula of the compound I is:

[0032]

[0033] Further, the molecular formula of the compound II is:

[0034]

[0035] Further, the molecular formula of the compound III is:

[0036]

[0037] Further, the predetermined conditions are: the oxygen pressure ...

specific Embodiment 1

[0042] The 3-picoline of 93g (1mol) is dissolved in the acetic acid of 1L, is made into 10% acetic acid solution, it is added the autoclave 10 of 2L, then adds catalyst (I) 25g (0.1mol, 10 % equivalent), 68% concentrated nitric acid 9g, airtight reaction kettle 10 and replace air with oxygen, under 1atm oxygen pressure, be warming up to 100 ℃, heat preservation reaction 2h, be down to room temperature, remove acetic acid under negative pressure, in the residue Add 200ml of water and 100ml of ethyl acetate, stir for 0.5h and filter a small amount of black insoluble matter, the filtrate is layered, the upper layer is the product layer, the quantitative analysis yield is 70%, the organic layer is precipitated to recover raw materials and catalysts.

specific Embodiment 2～5

[0044] The nicotine aldehyde product was prepared according to the operation process of the specific example 1, the difference is that the main catalyst and co-catalyst used, temperature, pressure, etc. are shown in Table 1, and the results are shown in Table 1.

[0045] Table 1

[0046]

[0047] The present invention also proposes a synthetic device that adopts a new method for synthesizing pymetrozine intermediate nicotinic aldehyde as described above, including a reaction kettle 10, a stirring shaft 20 and a vacuum distiller 30, and the stirring shaft 20 is provided with It is inside the reaction kettle 10 and is connected to the reaction kettle 10 in rotation. The vacuum distiller 30 is connected to the reaction kettle 10 and is arranged on the lower side of the reaction kettle 10 .

[0048] In this embodiment, the reaction kettle 10 is used as a reaction vessel, the stirring shaft 20 is used for mixing 3-picoline and acetic acid solution, and the vacuum distiller 30 is...

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Abstract

The invention discloses a novel pymetrozine intermediate nicotinaldehyde synthesis method. The method comprises the following steps: preparing a mixed solution; adding a main catalyst and a cocatalyst; and carrying out a reaction, cooling a reaction product, performing pressure reduced distillation and filtration to obtain a nicotinaldehyde solution. The invention further discloses synthesis equipment adopting the novel pymetrozine intermediate nicotinaldehyde synthesis method, the synthesis equipment comprises a reaction kettle, a stirring shaft and a reduced pressure distiller, the stirringshaft is arranged in the reaction kettle and is rotatably connected with the reaction kettle, the reduced pressure distiller is connected with the reaction kettle, and the reduced pressure distiller is connected with the reaction kettle and is located at the lower side of the reaction kettle. According to the present invention, the main catalyst and the co-catalyst are matched with each other, andthe experiment conditions are controlled, such that the process steps are simple and can be suitable for large-scale production, and the synthesis apparatus of the nicotinaldehyde synthesis method step is improved; the reaction kettle and the reduced pressure distiller are matched so as to improve the yield of the nicotinaldehyde; therefore, the product can be automatically produced, and the nicotinaldehyde can be produced on a large scale.

Description

technical field [0001] The invention relates to the technical field of synthetic technology of pesticide intermediates, in particular to a novel synthetic method and synthetic device of pymetrozine intermediate nicotinic aldehyde. Background technique [0002] Nicotinic aldehyde is a key intermediate in the synthesis of pymetrozine. The widely used process is to use fuming cyanide as the starting material and prepare nicotinic aldehyde by hydrogenation reduction of Raney nickel. The obvious defects of this process include the high price of starting material fuming cyanide. ;The reaction is easy to be over-reduced, generating a large number of by-products, which increases the amount of subsequent three wastes to be treated; the hydrogen used for the reduction is a flammable and explosive gas, and Raney nickel also has a high risk of fire, and high-level safety measures are required during production. In the prior art, an organic complex of cobalt and silver is used as a catal...

Claims

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Application Information

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IPC IPC(8): C07D213/48B01J31/02B01J19/18B01D3/00B01D3/10
CPCC07D213/48B01J31/0244B01J19/18B01D3/009B01D3/10B01J2231/70
Inventor 徐晓东王凯姜育田朱学军吴同文唐素荣傅晓东陈建国万金方于同锋王悦
Owner JIANGSU ANPON ELECTROCHEM
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