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Continuous synthesis method for methyl 3,3-dimethyl pentenoate

A technology for the synthesis of methyl pyretinate, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problem of continuous synthesis process report of methyl pyretinate and long reaction time , more tar, etc., to avoid high-temperature heating process, stable reaction yield, and reduced by-product tar

Active Publication Date: 2013-07-24
JIANGSU YANGNONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The literature "Research on the Synthesis of Methyl Cardyrinate" (Pesticide 1996, Issue 09) has carried out a literature review on the synthesis of Methyl Cardyrinate. In the prior art, the batch synthesis process is mainly used, which leads to long reaction time and long material time. Heated for a long time, there is a lot of tar in the rectification process, and the final product yield is only about 65-85%
[0006] Up to now, there is no continuous synthesis process report of methyl pyridinate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Trimethyl orthoacetate, anhydrous phosphoric acid and prenol are continuously entered into a tubular reaction at room temperature 25°C according to the molar ratio of trimethyl orthoacetate:anhydrous phosphoric acid:prenol=1:0.008:0.2 Mixing reaction in the reactor, the residence time is about 10 minutes, and the synthetic liquid of methyl bentinate in the intermediate state is generated. The synthetic liquid continuously enters the packing separation tower, and the temperature of the tower bottom is controlled at 120-130 ° C, and the top of the tower is 100-110 ° C. Produced methanol and excess trimethyl orthoacetate, the tower bottom liquid is then rectified to obtain the methyl perineate product, the gas chromatographic analysis content is 99.59%, and the yield is 90%.

Embodiment 2

[0024] Trimethyl orthoacetate, propionic acid and prenol are continuously fed into the one-pot reactor at room temperature 25°C according to the molar ratio of trimethyl orthoacetate:propionic acid:prenyl alcohol=1:0.008:0.2 Stir the reaction, the residence time is about 10 minutes, and generate the synthetic liquid of methyl bentinate in the intermediate state. The synthetic liquid continuously enters the packing separation tower. Methanol and excess trimethyl orthoacetate, and the tower bottom liquid was rectified to obtain the methyl perineate product, the gas chromatography analysis content was 99.53%, and the yield was 88.5%.

Embodiment 3

[0026] Trimethyl orthoacetate, 85% phosphoric acid and prenol are based on the molar ratio of trimethyl orthoacetate: 85% phosphoric acid: prenol=1: 0.01: 0.3 (85% phosphoric acid is calculated by the actual moles of phosphoric acid) , continuously enter a tubular reactor at room temperature 15°C to mix and react, and the residence time is about 15 minutes to generate an intermediate synthetic liquid of methyl bentinate. ℃, tower top 100-110 ℃, remove the by-product methanol and excess trimethyl orthoacetate, and then rectify the tower bottom liquid to obtain the methyl perineate product, the content of gas chromatography analysis is 99.5%, and the yield is 89.9%.

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PUM

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Abstract

The invention discloses a synthesis method for methyl-3,3-dimethyl-4-pentenoate. The method comprises the following steps of: A) continuously feeding trimethyl orthoacetate, a catalyst and 3-methyl-2-butenl-1-ol according to a molar ratio of 1:0.0005-0.02:0.1-0.5 into a tubular or kettle reactor, mixing and reacting for 5 to 60 minutes to produce methyl-3,3-dimethyl-4-pentenoate synthesis feed liquid at the temperature of between 0 and 40 DEG C; and B) continuously feeding the methyl-3,3-dimethyl-4-pentenoate synthesis feed liquid produced in the step A into a separating tower, removing methanol serving as a byproduct and excessive trimethyl orthoacetate, and rectifying tower bottom to obtain the methyl-3,3-dimethyl-4-pentenoate product. The synthesis method for the methyl-3,3-dimethyl-4-pentenoate in the invention has the advantages of high reaction speed, short period, a little of byproduct tar and simplicity and is particularly suitable for industrial large-scale production, and the reaction yield is stabilized at over 88 percent and product content is over 99.5 percent.

Description

technical field [0001] The invention relates to a method for synthesizing methyl pyridinate, in particular to a method for continuously synthesizing methyl carditinate. Background technique [0002] Methyl bentinate, the chemical name is 3,3 dimethyl-4-pentenoic acid methyl ester, the pure product is a colorless and transparent liquid with a special pungent smell, soluble in ethanol, ethyl acetate, ether and other organic solvents , insoluble in water; the structural formula is as follows: [0003] [0004] Methyl bentinate is an important chemical raw material. It is not only used in general organic synthesis, but also used as an intermediate in the synthesis of pyrethroid pesticides of fluorine, chlorine and bromine in the pesticide chemical industry. , occupies an important position, and was the first to be industrialized by the British Zeneca Company in the early 1970s. [0005] The literature "Research on the Synthesis of Methyl Cardyrinate" (Pesticide 1996, Issue ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/533C07C67/343
Inventor 戚明珠冯广军孙希祥蒋贤梅杨凡申于忠阳坤孙迎东张可
Owner JIANGSU YANGNONG CHEM
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