Method for synthesizing pesticide intermediate 3,3,3-trifluoro-2,2-dichloropropylaldehyde

A technology of dichloropropionaldehyde and trifluorotrichloroethane, which is applied in chemical instruments and methods, organic chemistry, preparation of halogenated hydrocarbons, etc., and can solve problems such as low yield of target products, difficulty in industrialization, low utilization rate of raw materials, etc. problem, to achieve the effect of high product yield, easy industrialization, and low raw material cost

Inactive Publication Date: 2018-12-04
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the methyl acrylate method has the disadvantages of few sources of raw materials and complicated operations; the trimethylchlorosilane method requires low temperature (-78°C) and nitrogen flow, and the operating conditions are harsh, making it difficult to realize industrialization; although the paraformaldehyde method has achieved One-pot method simplifies the process, but there are problems such as low utilization rate of raw materials, long reaction cycle and low yield of target product

Method used

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  • Method for synthesizing pesticide intermediate 3,3,3-trifluoro-2,2-dichloropropylaldehyde
  • Method for synthesizing pesticide intermediate 3,3,3-trifluoro-2,2-dichloropropylaldehyde
  • Method for synthesizing pesticide intermediate 3,3,3-trifluoro-2,2-dichloropropylaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Put 113.00 g of N,N-dimethylformamide, 113.00 g of styrene, 407.01 g of trifluorotrichloroethane, and 4.07 g of copper chloride powder into a 1L four-neck bottle, and heat up to 120°C for 6 hours of reaction. After the reaction was completed, gas spectrum quantitative analysis of the still material showed that styrene was 0.02%, butane was 47.11%, the conversion rate of styrene was 99.89%, and the yield of butane to styrene was 94.30%. The reaction solution was distilled under normal pressure and negative pressure, and the distillation fraction was 334.13g, which was applied mechanically; the temperature was lowered, and 8.20g of catalyst was recovered by filtration, which was applied mechanically; the filtrate was 320.12g, the butane content was 93.35%, and the yield of styrene was 93.20%.

Embodiment 2-4

[0036]The distillation fraction (containing trifluorotrichloroethane and N,N-dimethylformamide) and the recovered catalyst of Example 1 were applied mechanically. Taking set 1 as an example, put in 334.13g of the distilled fraction in Example 1, add 214.00g of trifluorotrichloroethane, 113.00g of styrene, then put in 8.21g of recovered catalyst and 0.20g of new catalyst, and heat up to 120°C for reaction 6 hours. After the heat preservation was completed, the temperature was lowered, and the aftertreatment was the same as that in Example 1 to obtain 8.62 g of recovered catalyst, 321.23 g of filtrate, 93.20% of butane content in the filtrate, and 94.70% of styrene yield for feeding.

Embodiment 3

[0037] Example 3 (set 2) The distilled fraction and recovered catalyst of example 2 (set 1) were used mechanically, new catalyst was supplemented, trifluorotrichloroethane and styrene were added, and the reaction was carried out at 120° C. for 6 hours.

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Abstract

The invention belongs to the technical field of organic chemical engineering and relates to a method for preparing an important intermediate, i.e., 3,3,3-trifluoro-2,2-dichloropropylaldehyde of a halogen-containing pyridine organic compound. More specifically, the method disclosed by the invention comprises the step of subjecting 1,1,1-trifluorotrichloroethane and styrene, which serve as raw materials, to addition, dehalogenation, ozonation and reduction reactions, thereby synthesizing the important intermediate, i.e., 3,3,3-trifluoro-2,2-dichloropropylaldehyde of chlorfluazuron, fluazuron, Haloxyfop and Fluazinam. The total yield is stabilized to 70% or more, and the product purity is 99% or more. According to the method, the process is clean, the raw material cost is low, the product purity is high, and the industrial production is easy to achieve.

Description

technical field [0001] The present invention belongs to the technical field of organic chemical industry, relates to the preparation method of the important intermediate 3,3,3-trifluoro-2,2-dichloropropanal of halogen-containing pyridine organic compounds, more specifically, relates to a kind of ,1,1-Trifluorotrichloroethane and styrene were used as raw materials to synthesize acetamicarb, pyridoxuron, haloxyfop, and fluazinam through addition, dehalogenation, ozonation, and reduction reactions. The intermediate 3,3,3-trifluoro-2,2-dichloropropanal has a stable total yield of over 70%, and a product purity of over 99%. The invention has clean process, low raw material cost, high product purity and easy realization of industrialized production. Background technique [0002] 3,3,3-Trifluoro-2,2-dichloropropanal (CAS No.: 82107-24-2, hereinafter referred to as "trifluorodichloropropanal") can be prepared by ring-closing reaction to prepare 2,3-dichloro- 5-trifluoromethylpyrid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/14C07C47/54C07C45/40C07C22/08C07C17/275C07C17/25
CPCC07C17/25C07C17/275C07C45/40C07C22/08C07C47/14C07C47/54
Inventor 王根林丁克鸿徐林王刚殷恒志王铖戚明甫许越
Owner JIANGSU YANGNONG CHEM GROUP
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