Preparation method for 2,6-dichloro-4-fluorobenzaldehyde

A technology of fluorobenzaldehyde and dichloride, which is applied in the field of preparation of 2,6-dichloro-4-fluorobenzaldehyde, can solve problems such as application limitation, low yield of benzaldehyde, pollute the environment, etc., and achieves simple operation, raw material Easy to obtain, high yield effect

Inactive Publication Date: 2018-08-03
珠海奥博凯生物医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method not only pollutes the environment but also has a low yield of ...

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  • Preparation method for 2,6-dichloro-4-fluorobenzaldehyde
  • Preparation method for 2,6-dichloro-4-fluorobenzaldehyde

Examples

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Embodiment 1

[0018] (1) Preparation of isopropylmagnesium chloride Grignard reagent: first add 20 mL of tetrahydrofuran and 3 g of 2-chloropropane into a 50 mL one-necked flask and stir to make a solution, and set aside. Under the protection of nitrogen, in a 50mL dry three-necked flask, add 1.1g of magnesium chips, a small amount of 2-chloropropane, and a small amount of tetrahydrofuran solvent, raise the temperature to 30-40°C, and initiate the reaction with bromoethane. Then the tetrahydrofuran solution of 2-chloropropane was added dropwise, and after the dropwise addition was completed, an insulation reaction was carried out, and the concentration of the obtained isopropylmagnesium chloride Grignard reagent was 1.7 mol / L.

[0019] (2) Grignard exchange: under the protection of nitrogen, add 10 g of 2,6-dichloro-4-fluoroiodobenzene and 20 ml of tetrahydrofuran into a 100 ml dry three-necked flask. Cool down to 0°C, slowly add the above-prepared isopropylmagnesium chloride Grignard reage...

Embodiment 2

[0023] (1) Preparation of isopropylmagnesium chloride Grignard reagent: first add 20 mL of tetrahydrofuran and 3 g of 2-chloropropane into a 50 mL one-necked flask and stir to make a solution, and set aside. Under the protection of nitrogen, in a 50mL dry three-necked flask, add 1.1g of magnesium chips, a small amount of 2-chloropropane, and a small amount of tetrahydrofuran solvent, raise the temperature to 30-40°C, and initiate the reaction with bromoethane. Then the tetrahydrofuran solution of 2-chloropropane was added dropwise, and after the dropwise addition was completed, an insulation reaction was carried out, and the concentration of the obtained isopropylmagnesium chloride Grignard reagent was 1.7 mol / L.

[0024] (2) Grignard exchange: under the protection of nitrogen, add 10 g of 2,6-dichloro-4-fluoroiodobenzene and 20 ml of tetrahydrofuran into a 100 ml dry three-necked flask. Cool down to -20°C, slowly add the above-prepared isopropylmagnesium chloride Grignard rea...

Embodiment 3

[0028] (1) Preparation of isopropylmagnesium chloride Grignard reagent: first add 20 mL of tetrahydrofuran and 3 g of 2-chloropropane into a 50 mL one-necked flask and stir to make a solution, and set aside. Under the protection of nitrogen, in a 50mL dry three-necked flask, add 1.1g of magnesium chips, a small amount of 2-chloropropane, and a small amount of tetrahydrofuran solvent, raise the temperature to 30-40°C, and initiate the reaction with bromoethane. Then the tetrahydrofuran solution of 2-chloropropane was added dropwise, and after the dropwise addition was completed, an insulation reaction was carried out, and the concentration of the obtained isopropylmagnesium chloride Grignard reagent was 1.7 mol / L.

[0029] (2) Grignard exchange: under nitrogen protection, 7.4 g of 2,6-dichloro-4-fluoroiodobenzene and 20 ml of tetrahydrofuran were added to a 100 ml dry three-necked flask. Cool down to 10°C, slowly add the above-prepared isopropylmagnesium chloride Grignard reage...

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method for 2,6-dichloro-4-fluorobenzaldehyde. The preparation method comprises the following steps: selecting commercially available 1,3-dichloro-2-fluoro-5-iodobenzene as a raw material; under a low-temperature condition, carrying out Grignard exchange reaction on 2,6-dichloro-4-fluoroiodobenzene and isopropylmagnesium chloride to prepare the Grignard reagent of phenylmagnesium chloride; carrying out formylation reaction on the obtained Grignard reagent of phenylmagnesium chloride andN,N-dimethylformamide; after hydrolysis is carried out through diluted hydrochloric acid, obtaining a 2,6-dichloro-4-fluorobenzaldehyde crude product; finally, purifying to obtain a 2,6-dichloro-4-fluorobenzaldehyde finished product. The method has the advantages of abundant raw material, high reaction purity yield, stable technical condition and simpleness in operation, is suitable for mass production and provides a new thought and method for preparing the 2,6-dichloro-4-fluorobenzaldehyde.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2,6-dichloro-4-fluorobenzaldehyde. Background technique: [0002] 2,6-Dichloro-4-fluorobenzaldehyde is a light yellow crystal and is a chemical intermediate with a wide range of uses, widely used in the synthesis of pharmaceuticals and other fine chemical products. The traditional method of synthesizing benzaldehyde is toluene halogenation hydrolysis, which is to produce benzaldehyde through toluene toluene chlorination reaction and saponification reaction. This method not only pollutes the environment but also has a low yield of benzaldehyde, and the product contains halide ions, which limits its application. Therefore, it is of great significance to seek an efficient and clean synthesis route of benzaldehyde. Invention content: [0003] The technical problem to be solved by the present invention is to provide a method for preparing 2,6-dic...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C47/55
CPCC07C45/004C07C45/455C07F3/02C07C47/55
Inventor 曾梦静周运芬杨春朋
Owner 珠海奥博凯生物医药技术有限公司
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