Preparation method of carboxylic ester compounds

An ester compound and compound technology, applied in the field of compound synthesis, can solve the problems of low catalyst activity, reduced production capacity, difficult to handle, etc., and achieve the effects of high catalyst activity, reduced environmental protection pressure, and less side reactions

Pending Publication Date: 2020-05-08
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the above process, the addition process uses cuprous chloride and ethanolamine, the catalyst activity is low, and the reaction time is as long as 20 hours. After the addition reaction is completed, the catalyst needs to be settl

Method used

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  • Preparation method of carboxylic ester compounds
  • Preparation method of carboxylic ester compounds
  • Preparation method of carboxylic ester compounds

Examples

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Example Embodiment

[0026] The present invention provides a method for preparing a carboxylic acid ester compound, including the following steps:

[0027] a) Under the action of a catalyst, the compound of formula (A) and the compound of formula (B) react to obtain the carboxylic acid ester compound of the structure represented by formula (C);

[0028]

[0029]

[0030] In formula (A)~(C), R 1 Selected from C 1 ~C 2 Alkyl, R 2 ~R 5 Independently selected from hydrogen, halogen, C 1 ~C 3 Alkyl or C 1 ~C 3 Haloalkyl

[0031] The catalyst includes azobisisobutyronitrile and / or peroxy catalyst.

[0032] In the preparation method provided by the present invention, the structure compound of formula (A) and the structure compound of formula (B) are used as reaction materials. Wherein, R in the compound of formula (A) 1 The group is methyl or ethyl, that is, the compound of the formula (A) can be methyl bentinate or ethyl bentinate; R in the compound of the formula (B) 2 ~R 5 Groups are independently selected fr...

Example Embodiment

[0044] Example 1

[0045] Synthesize carboxylic acid ester compounds according to the following chemical equation:

[0046]

[0047] The specific process includes:

[0048] 1) Under the protection of nitrogen, add 145.1g methyl bentinate to a 500ml autoclave, close the autoclave tightly, heat up to 60℃, pump in 0.71g tert-butyl peroxyneodecanoate and 283.4g trifluoroacetate through the feeding port The trichloroethane mixture is pumped in after 2h. Continue the incubation reaction for 4h.

[0049] 2) Cool down to 30°C, transfer the reaction solution to a four-necked flask, and recover excess trifluorotrichloroethane under reduced pressure to obtain 330.2 g of product. The product content is 99.0% by GC analysis, and the yield is 99.2%.

[0050] The product prepared in this example was analyzed by gas chromatography and mass spectrometry, and the chromatographic analysis results were as follows figure 1 And Table 1, figure 1 Is the chromatogram provided in Example 1 of the present inve...

Example Embodiment

[0053] Example 2

[0054] Synthesize carboxylic acid ester compounds according to the following chemical equation:

[0055]

[0056] The specific process includes:

[0057] 1) Under nitrogen protection, add 156.2g ethyl bentinate to a 500ml autoclave, close the autoclave tightly, heat up to 40°C, pump 2.84g azobisisobutyronitrile and 169.5g dichloromethane through the feeding port Liquid, the pumping ends after 2h. Continue the incubation reaction for 4h.

[0058] 2) The temperature was lowered to 30°C, the reaction solution was transferred to a four-necked flask, and excess dichloromethane was recovered under reduced pressure to obtain 241.2 g of product. The product content was 98.0% by GC analysis and the yield was 98.1%.

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Abstract

The invention belongs to the technical field of compound synthesis, and particularly relates to a preparation method of carboxylic ester compounds. A compound having a structure represented by formula(A) reacts with a compound having a structure represented by formula (B) under the action of a catalyst to obtain the carboxylic ester compounds having a structure represented by formula (C); in theformulas (A)-(C), R1 is selected from C1-C2 alkyl groups; R2 to R5 are independently selected from hydrogen, halogen, C1-3 alkyl groups or C1-3 halogenated alkyl groups; and the catalyst comprises azodiisobutyronitrile and/or a peroxide catalyst. The compound of formula (A) and the compound of formula (B) are used as reaction raw materials and directly react under the action of the specific catalyst to obtain the carboxylic ester compounds. The method has the advantages of high catalytic activity, simple process flow, low post-treatment difficulty and high production efficiency, can avoid thegeneration of three wastes, and conforms to the environmental protection requirements.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a preparation method of carboxylic acid ester compounds. Background technique [0002] Halogen-3,3-dimethyl-heptane carboxylate compounds are synthetic compounds of lambda-cyhalothrin, tefluthrin, resmethrin, phenothrin, permethrin, cypermethrin, bromemethrin Important intermediates of pyrethroids such as permethrin and tetrabromothrin. The global sales of pyrethroid products rose rapidly from US$2.08 billion in 2009 to US$3.16 billion in 2014, with a compound annual growth rate of 8.7%. From the perspective of the distribution of global insecticide products, the market share of pyrethroids is 17.0%, second only to neonicotinoid insecticides. From the perspective of the scale distribution of permethrin products, in 2015, the global sales volume was mainly agricultural permethrin, among which the sales of beta-cyhalothrin (Kung Fu permethrin) reached 630 m...

Claims

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Application Information

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IPC IPC(8): C07C67/307C07C69/63
CPCC07C67/307C07C69/63Y02P20/584
Inventor 李志清绳敏姚红霞徐安
Owner SHANDONG WEIFANG RAINBOW CHEM
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