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Method for producing 2, 4-dinitrobenzene methyl ether and 2, 4- dinitrophenol simultaneously

A technology of dinitroanisole and dinitrophenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as harsh process conditions, difficult operation, and long reaction time

Inactive Publication Date: 2012-03-28
山东昌邑灶户盐化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2,4-Dinitroanisole and 2,4-Dinitrophenol are intermediates for the preparation of dyes and medicines. Currently, there are disadvantages in the synthesis of 2,4-Dinitroanisole: the amount of solvent methanol is large, Generally, it is 15 to 20 times the molar amount of 2,4-dinitrochlorobenzene; the reaction time is as long as 10 hours; the process conditions are harsh and the operation is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 9.6 g (0.3 mol) of methanol and 20.3 g (0.1 mol) of 2,4-dinitrochlorobenzene to the reaction flask in sequence, heat until the 2,4-dinitrochlorobenzene is completely dissolved, start stirring, 5-10 Add 14 g of sodium hydroxide solution with a mass concentration of 10% (the molar weight of sodium hydroxide is 0.105 mol) dropwise within 1 min, continue heating to reflux, and react for 2 hours at 70 ° C, distill methanol, and then add 6 mL of water, adjust the pH to 8-10 with a 10% sodium hydroxide solution, cool to room temperature, filter, wash twice with a sodium hydroxide aqueous solution with a pH of 8-10, combine the filtrate and washing liquid, and filter cake Then wash with cold water until the pH is 7, and dry to obtain 8.9 g of 2,4-dinitroanisole, the yield is 45% based on 2,4-dinitrochlorobenzene, and the melting point is 93-95°C.

[0022] The above filtrate was adjusted to pH 2.5-4.5 with 10% hydrochloric acid, cooled to 20 °C, crystallized for 1 hour, filt...

Embodiment 2

[0024] Add 16g (0.5 mol) of methanol and 20.3 g (0.1 mol) of 2,4-dinitrochlorobenzene to the reaction flask in sequence, heat until 2,4-dinitrochlorobenzene is completely dissolved, and start stirring for 5-10 min Add 42 g of sodium hydroxide solution with a mass concentration of 30% (the molar weight of sodium hydroxide is 0.105 mol), continue heating to reflux, and react at 62 °C for 3 hours, then distill off methanol, and then add 20 mL water, adjust the pH to 8-10 with 30% sodium hydroxide solution, drop to room temperature, filter, wash twice with sodium hydroxide aqueous solution with pH 8-10, combine the filtrate and lotion, and wash the filter cake with cold water until The pH is 7 and dried to obtain 8.9 g of 2,4-dinitroanisole. The yield is 60.6% based on 2,4-dinitrochlorobenzene, and the melting point is 93-95°C.

[0025] The above filtrate was adjusted to pH 2.5-3.5 with 20% hydrochloric acid, cooled to 5 °C, crystallized for 1 hour, filtered, washed with cold wate...

Embodiment 3

[0027] Add 25.6 g (0.8 mol) of methanol and 20.3 g (0.1 mol) of 2,4-dinitrochlorobenzene to the reaction flask in sequence, heat until 2,4-dinitrochlorobenzene is completely dissolved, and start stirring, 5 to 10 Add 10.5 g of 40% sodium hydroxide solution dropwise within 1 min (the molar weight of sodium hydroxide is 0.105 mol), continue heating to reflux, and react at 56°C for 5 hours, then distill off the methanol, then add 24 mL of water, and use Adjust the pH to 8-10 with 30% sodium hydroxide solution, cool down to room temperature, filter, wash 3 times with aqueous sodium hydroxide solution with a pH of 8-10, combine the filtrate and washing liquid, and wash the filter cake with cold water until the pH is 7 , and dried to obtain 15.8 g of 2,4-dinitroanisole, calculated as 2,4-dinitrochlorobenzene, the yield was 80%, and the melting point was 93-95°C.

[0028] The above filtrate was adjusted to pH 2.5-4.5 with 35% hydrochloric acid, cooled to 10°C, crystallized for 1 hour...

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Abstract

The invention discloses a method for producing 2, 4- dinitrobenzene methyl ether and 2, 4-dinitrophenol simultaneously, which is characterized by comprising the following steps: feeding and reacting stage: adding methanol and 2, 4- dinitro chloro benzene into a reaction device, heating until the 2, 4- dinitro chloro benzene is complately dissolved, and dripping sodium hydroxide water solution for reaction, so as to obtain the mixture of 2, 4- dinitrobenzene methyl ether and 2, 4- dinitrophenol; extracting 2, 4- dinitrobenzene methyl ether; obtaining methanol through steaming after reaction, adding water, regulating pH, lowering the temperature and suction filtering, washing a filter cake through water, and then drying, so as to obtain 2, 4- dinitrobenzene methyl ether; and extracting 2, 4- dinitrophenol; regulating the pH value of obtained filter liquor, cooling and crystallizing, washing through water, filtering, and drying so as to obtain 2, 4- dinitrophenol. The process is simple, the reaction time is short, the efficiency is high, the use level of the methanol can be effectively reduced, and the toxicity is lowered.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for simultaneously producing 2,4-dinitroanisole and 2,4-dinitrophenol. Background technique [0002] 2,4-Dinitroanisole and 2,4-Dinitrophenol are intermediates for the preparation of dyes and medicines. Currently, there are disadvantages in the synthesis of 2,4-Dinitroanisole: the amount of solvent methanol is large, Generally, it is 15 to 20 times the molar amount of 2,4-dinitrochlorobenzene; the reaction time is as long as 10 hours; the process conditions are harsh and the operation is difficult. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for simultaneously producing 2,4-dinitroanisole and 2,4-dinitrophenol with simple process, less solvent methanol consumption and short reaction time. [0004] In order to solve the problems of the technologies described above, the technical soluti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/37C07C205/23
Inventor 付忠东高建伟解德水万克玲梁足培
Owner 山东昌邑灶户盐化有限公司
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