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Preparation method of bifenthrin insecticide intermediate

A solvent and catalyst technology, applied in the field of pesticides, can solve problems such as safety risks, low yields, and high costs

Pending Publication Date: 2021-09-24
湖南华腾制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of the above-mentioned preparation method of bifenthrin intermediate D, it has technical problems of low yield, high cost, and safety risk. One aspect of the present invention is to provide a preparation method of bifenthrin intermediate D, which The method has the characteristics of high yield, low cost, good safety and suitable for industrial scale-up

Method used

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  • Preparation method of bifenthrin insecticide intermediate
  • Preparation method of bifenthrin insecticide intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1 Preparation of Compound B

[0049]

[0050] THF (50 mL), Compound A (20g) and magnesium powder (194 g) were added to a 3L three flask (194 g), and 1.2-dibromoethane (1.5 mL) was added, and the mixture was stirred to 40 ° C to initiate the reaction, slowly dropped the formulated compound. A of the tetrahydrofuran solution (980 g of Compound A is dissolved in 1.2 L tetrahydrofuran), and then stirred at 80 ° C after drying 1 h. Cooling, saving for use.

Embodiment 2

[0051] Example 2 Preparation of Compound D

[0052]

[0053] Add compound C (2 kg) and MnCl to 10L reactor 2 (100 g), nitrogen replacement twice, warmed to 80 ° C to 96 ° C, and slowly added a compound B reaction (3L) obtained according to the preparation method in Example 1. Stirring was continued at 85 ° C after drying. After the reaction was complete, the reaction solution was poured into ice hydrochloric acid (3 mol / L, 2.8L), extracted twice with DCM (0.7 L * 2), combined with organic phases, reverse washing with water (0.7L), anhydrous sulfuric acid Sodium dried over, concentrated under reduced pressure, resulting in compound D, 0.56 kg, two-step income rate: 45%, purity 98.5%.

[0054] HNMR (CD 3 OD) PPM: 7.44-7.40 (m, 2H), 7.37-7.34 (m, 2H), 7.26-7.24 (D, 2H), 7.20-7.16 (T, 1H), 7.12-7.10 (D, 1H), 2.25 (s, 3h).

Embodiment 3

[0055] Example 3 Preparation of Compound D

[0056] Compound C (2 kg) and PD / C (100 g) were added to a 10L reaction kettle, and the nitrogen was replaced twice, and the compound B reaction solution obtained by slowly dropped according to the preparation method in Example 1 was added to 80-96 ° C. . After stirring at 85 ° C, stir it at 85 ° C. After the reaction was complete, the reaction solution was poured into ice hydrochloric acid (3 mol / L, 2.8L), DCM (0.7 L * 2) was extracted twice, combined with organic phases, wash it once with water (0.7L), dry alhydrate sodium sulfate , Concentrated under reduced pressure, resulting in 0.50 kg of compound D, two-step consolidation yield: 33.5%, purity: 98.6%.

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Abstract

The invention relates to a preparation method of a bifenthrin insecticide intermediate, and belongs to the field of pesticides. The preparation method comprises the following steps: by taking cheap 2, 6-dichlorotoluene as a starting material, carrying out Grignard reaction and coupling reaction to obtain a bifenthrin insecticide intermediate D. The method has the characteristics of high yield, low cost, good safety and suitability for industrial amplification.

Description

Technical field [0001] The present invention relates to the field of pesticide, and more particularly to a method for preparing a biphenyl pesticide insecticide intermediate. Background technique [0002] BiFENTHRIN, CAS: 82657-04-3, is one of the new types of pegs and pegs, and is widely used in countries around the world. This product has the characteristics of strong knocking, broad-spectrum, efficient, rapid, long and effective, with triburn and stomach toxic effects, no intraction. Can be used to prevent cotton bollworm, red bell, tea, tea caterpillar, apple or hawthorn red spider, peach fresh food aphid, vegetable, vegetable green moth, citrus, citrus, citrus, citrus, moth, etc. Its chemical structural formula is as shown in Formula i: [0003] [0004] Among them, 3-chlorine-2-methylbenzene is a key intermediate of biphenyl chryney ester, as shown in the following formula D: [0005] [0006] Synthesis of intermediate D of Intermediate D disclosed in U.S. Patent No. 4,...

Claims

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Application Information

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IPC IPC(8): C07C17/263C07C25/18C07F3/02
CPCC07C17/2632C07F3/02C07C25/18
Inventor 金艳娟田涛陈仔玲李斌陈闽余健何光明
Owner 湖南华腾制药有限公司
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