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Synthetic method of pesticide intermediate 2-chloro-4-formyl valeronitrile

A technology of formylvaleronitrile and dimethylformamide is applied in the field of synthesizing 2-chloro-4-formylvaleronitrile, and can solve the problems of great harm to the environment and operators, complicated preparation process and high quality requirements

Active Publication Date: 2015-08-26
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the EP0162464 patent uses morpholine and propionaldehyde as raw materials to synthesize 1-morpholinopropene, which reacts with 2-chloroacrylonitrile and hydrolyzes to obtain the precursor 2-chloro-4-formylvaleronitrile. DMF is the solvent and catalyst, hydrogen chloride gas is the initiator, successfully synthesized 2-chloro-5-picoline, however, the preparation process of 1-morpholinopropene and 2-chloroacrylonitrile is more complicated and requires high quality , in addition, 2-chloroacrylonitrile is a highly toxic substance, which is very harmful to the environment and operators

Method used

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  • Synthetic method of pesticide intermediate 2-chloro-4-formyl valeronitrile

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 500ml four-necked round-bottom reaction flask, add 100g of dichloromethane and 0.5g of DMF, purge the system with nitrogen, control the temperature in a water bath, and add 58g of propionaldehyde (1mol) dropwise at 10°C. Chlorine gas is introduced at a flow rate of 16-17L / hr, and the dripping time is 2hr. After the dripping is completed, continue to pass chlorine gas, and keep warm for 2hrs. The liquid is under normal pressure, rectified to recover dichloromethane, and when the liquid temperature reaches 80°C, stop collecting materials. Under the vacuum condition of -0.055MPa, the residue in the still was simply distilled, and 81.8g of distillates with a temperature of 64-66°C were collected.

[0032] Gas spectrum analysis product content is 99.0%, appearance is colorless and transparent, and the yield of 2-chloropropionaldehyde is 87.5%.

Embodiment 2-4

[0034] On the basis of Example 1, tetraethylammonium chloride, triethylamine hydrochloride, and tetramethylammonium chloride were used as catalysts respectively, and other conditions remained unchanged. The obtained results are shown in Table 1.

[0035] The impact of different catalysts in table 1 on the yield of 2-chloropropionaldehyde

[0036]

Embodiment 5-7

[0038] The methylene chloride recovered in Example 1 is applied mechanically, and other conditions are the same as in Example 1. The obtained results are shown in Table 2.

[0039] Table 2 applies mechanically to the impact of reclaiming dichloromethane on 2-chloropropionaldehyde

[0040]

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Abstract

The invention belongs to the technical field of organic chemical industry, and relates to a synthetic method of a precursor of an imidacloprid pesticide intermediate 2-chloro-4-formyl valeronitrile. According to the synthetic method, propionaldehyde and chlorine gas are taken as initial raw materials, 2-chloride propyl aldehyde is prepared via substitution, and catalytic addition with acrylonitrile is carried out so as to obtain 2-chloro-4-formyl valeronitrile via synthesis, and total yield is stabilized to be higher than 70%. According to the synthetic method, chlorine substitution and addition two-step reaction is adopted, 2-chloro-4-formyl valeronitrile is prepared, the synthetic method is simple in technological process, low in production cost, and low in equipment investment, and is suitable for industrialized production, and raw material recovery is convenient to realize.

Description

technical field [0001] The present invention belongs to the technical field of organic chemical industry, relates to a kind of synthetic method of the precursor 2-chloro-4-formyl valeronitrile of imidacloprid pesticide intermediate, more specifically, relates to a kind of with propionaldehyde and chlorine gas as starting raw material, Instead of preparing 2-chloropropionaldehyde, and then catalytic addition reaction with acrylonitrile, 2-chloro-4-formylvaleronitrile was synthesized, and the total yield was stable above 70%. In the present invention, 2-chloro-4-formylvaleronitrile can be obtained through two-step reaction of chlorine substitution and addition, which has the characteristics of simple process flow, low production cost, less investment in equipment and easy recycling of raw materials, etc., and is suitable for industrialization Production. Background technique [0002] 2-Chloro-5-methylpyridine (CMP for short) is an important intermediate for the synthesis of n...

Claims

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Application Information

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IPC IPC(8): C07C255/17C07C253/30C07D213/61
Inventor 王根林申明稳丁克鸿王刚刘补娥
Owner JIANGSU YANGNONG CHEM GROUP
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