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A kind of new synthetic method of pymetrozine intermediate nicotinic aldehyde

A synthesis method and pymetrozine technology are applied in the field of synthesis technology of pesticide intermediates, can solve the problem that the synthesis technology of nicotinic aldehyde cannot be applied to large-scale production and the like, and achieve the effect of simple process steps

Active Publication Date: 2022-05-13
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 nicotinic aldehyde synthesis process cannot be applied to large-scale production, the present invention proposes a new synthesis method of pymetrozine intermediate nicotinic aldehyde

Method used

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  • A kind of new synthetic method of pymetrozine intermediate nicotinic aldehyde
  • A kind of new synthetic method of pymetrozine intermediate nicotinic aldehyde
  • A kind of new synthetic method of pymetrozine intermediate nicotinic aldehyde

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preparation example Construction

[0022] A new method for synthesizing pymetrozine intermediate nicotinaldehyde, comprising the steps of:

[0023] S101: making 10-50% acetic acid solution with 3-picoline;

[0024] S102: adding 1-10% by mass of the main catalyst and 1%-50% by mass of the co-catalyst into the solution;

[0025] 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.

[0026] Further, the main catalyst is a nitrogen hydroxyl compound, including compound I, compound II and compound III.

[0027] Further, the molecular formula of the compound I is:

[0028]

[0029] Further, the molecular formula of the compound II is:

[0030]

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

[0032]

[0033] Further, the predetermined conditions are: the oxygen pressure is 1-10 atm, and the reaction is at 20-100° C. for 2...

specific Embodiment 1

[0037] The 3-picoline of 93g (1mol) is dissolved in the acetic acid of 1L, is made into 10% acetic acid solution, it is added into the autoclave 10 of 2L, then in still, add catalyst (I) 25g (0.1mol, 10 % equivalent), 9 g of 68% concentrated nitric acid, sealed reaction kettle 10 and replaced the air with oxygen, under 1 atm oxygen pressure, raised the temperature to 100 ° C, kept the temperature for 2 hours, cooled down to room temperature, removed acetic acid under negative pressure, and poured into 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

[0039] The nicotine aldehyde product was prepared according to the operation process of the specific example 1, the difference is that the type of main catalyst and co-catalyst used, temperature, pressure, etc. are shown in Table 1, and the results are shown in Table 1.

[0040]

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Abstract

The invention discloses a new method for synthesizing nicotinic aldehyde, an intermediate of pymetrozine, which comprises the following steps: preparing a mixed solution; adding a main catalyst and a cocatalyst; reacting, cooling, vacuum distillation, and filtering to prepare a nicotinic aldehyde solution, Improve the steps of the synthetic method of nicotinic aldehyde, use the cooperation of the main catalyst and the co-catalyst, and control the experimental conditions, so that the process steps are simple and can be adapted to large-scale production, and the synthetic device of the synthetic method step of the nicotinic aldehyde is improved, By using the cooperation of the reaction kettle and the vacuum distiller, the product can be produced automatically, and then the nicotine aldehyde 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 new method for synthesizing nicotinic aldehyde, an intermediate of pymetrozine. 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 catalyst to direc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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