Synthetic process for 2,4-dinitroanisole

A technology of dinitroanisole and synthesis process, which is applied to the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., which can solve problems such as environmental hazards, increased reaction water volume, and reduced yield, and achieve improved reaction Selectivity, reduction of environmental pollution, and reduction of treatment costs

Active Publication Date: 2013-11-20
ZHEJIANG DIBANG CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] In the reported process method, liquid caustic soda is continuously added dropwise in the reaction. Due to the strong alkalinity of liquid caustic soda, at a certain temperature, the hydrolysis of 2,4-dinitrochlorobenzene is accelerated, and the by-product 2,4-dinitrochlorobenzene The increase of the content of base phenol makes the purity of 2,4-dinitroanisole decrease, and the yield also decreases; at the same time, the addition of liquid caustic soda increases the amount of reaction water, produces a large amount of waste water after the reaction, and the mother liquor cannot be continuously recycled, and then A large amount of waste water is produced, causing great harm to the environment, and at the same time, the cost of the post-treatment process also increases accordingly

Method used

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  • Synthetic process for 2,4-dinitroanisole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add 32g (1mol) of methanol into a 150mL four-neck flask, slowly add 16g (0.4mol) of solid sodium hydroxide (0.4mol) and 0.8g (0.02mol) of magnesium oxide under stirring, and control the temperature not to exceed 65°C until the solids are completely dissolved Obtain methanol lye for use.

[0028] (2) Add 45g (1.41mol) of methanol into a 500mL four-neck flask, add 81g (0.4mol) of 2,4-dinitrochlorobenzene under stirring, and heat until 2,4-dinitrochlorobenzene is completely dissolved. Drop the methanol lye obtained in step (1) within 30 minutes, and keep it at 70°C for 3 hours. After cooling to room temperature, suction filtration after the crystals were precipitated, 83 g of the filtrate was collected, and the filtrate was distilled under reduced pressure to obtain 45 g of the mother liquor. The filter cake was washed with water at 30°C until it was neutral, the washing liquid was collected, and the filter cake was dried to obtain 76.4 g of 2,4-dinitroanisole, the yi...

Embodiment 2

[0032] According to the method described in Example 1, 40 g (1.25 mol) of methanol was added in step (1).

[0033] In step (2), 50 g (1.56 mol) of methanol was added, and the reaction was carried out at 72° C. for 5 hours. Obtain 96g of filtrate, 58g of mother liquor after filtrate is distilled under reduced pressure, 76.0g of 2,4-dinitroanisole, take 2,4-dinitrochlorobenzene, the yield is 95.8%, liquid chromatography detects purity 99.8%. 1.77 g of 2,4-dinitrophenol was obtained, calculated as 2,4-dinitrochlorobenzene, the yield was 2.4%, and the purity by liquid chromatography was 99.0%.

[0034]Mother liquor application: According to the method described in Example 1, 40 g (1.25 mol) of methanol was added in step (3).

[0035] In step (4), 58 g of mother liquor and 25.6 g (0.8 mol) of methanol were added, and the mixture was incubated at 72° C. for 5 hours. 108 g of filtrate and 76.5 g of 2,4-dinitroanisole were obtained, calculated as 2,4-dinitrochlorobenzene, the yield...

Embodiment 3

[0037] According to the method described in Example 1, 44.8 g (1.4 mol) of methanol was added in step (1).

[0038] In step (2), 57.6 g (1.8 mol) of methanol was added, and the reaction was carried out at 75° C. for 6 hours. Obtain filtrate 110g, the mother liquor 70g after filtrate is distilled under reduced pressure, obtain 2,4-dinitroanisole 75.3g, calculate with 2,4-dinitrochlorobenzene, yield is 95%, liquid chromatography detects 99.5% purity. 2.12 g of 2,4-dinitrophenol was obtained, calculated as 2,4-dinitrochlorobenzene, the yield was 2.88%, and the purity by liquid chromatography was 98.3%.

[0039] Mother liquor application: According to the method described in Example 1, 44.8 g (1.4 mol) of methanol was added in step (3).

[0040] In step (4), 70 g of mother liquor and 28.8 g (1.8 mol) of methanol were added, and the mixture was incubated at 75°C for 6 hours. Obtain filtrate 105g, the mother liquor 70g after filtrate is distilled under reduced pressure, obtain 2,...

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Abstract

The invention discloses a synthetic process for 2,4-dinitroanisole. The synthetic process comprises the following steps of: heating and dissolving composite inorganic base into methanol to obtain a methanol alkali solution, then dropwise adding the methanol alkali solution into a methanol solution containing the 2,4-dinitroanisole to react, after finishing the reaction, carrying out cooling crystallization on the obtained reaction liquid, filtering to obtain a filter cake and filter liquid, washing the filter cake by utilizing water of 30-35 DEG C to obtain solids and washing liquid, and drying the obtained solids to obtain 2,4-dinitroanisole; and regulating the pH of the obtained washing liquid to be 2-4, and carrying out the cooling crystallization, filtering, water washing and drying to obtain 2,4-dinitrophenol. The synthetic process has the advantages that the purity and yield of the 2,4-dinitroanisole are improved, the water volume of mother liquid is effectively reduced, and the mother liquid can be continuously and mechanically applied after being processed, is accordant with industrial production requirements and can be used for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and in particular relates to a synthesis process of 2,4-dinitroanisole. Background technique [0002] 2,4-Dinitroanisole (CAS: 119-27-7) is an important fine chemical intermediate, which can be used in fine chemical fields such as dyes, medicines and pesticides. The traditional 2,4-dinitroanisole is mainly prepared by using methanol as a solvent, using an inorganic base as an acid-binding agent to react with 2,4-dinitrochlorobenzene, wherein methanol is both a raw material and a reaction solvent , considering cost, catalytic efficiency and availability, the inorganic base used in the reaction is usually an aqueous solution of sodium hydroxide. Generally need a large amount of methanol to make solvent in the technology that has been reported at present, and use the aqueous solution of sodium hydroxide to bring a large amount of water in the reaction, the reaction time is long, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/37C07C201/12
Inventor 徐万福刘伟周海滨
Owner ZHEJIANG DIBANG CHEM
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