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A technology of ethylaminophenol and xylene, which is applied in the field of synthesis of intermediate compounds, can solve problems such as troublesome handling, and achieve the effects of long production process, low boiling point and high risk
Pending Publication Date: 2020-12-29
安徽绿色谷创客空间股份有限公司 +1
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[0004] In order to solve the above problems, the object of the present invention is to provide a method for synthesizing m-diethylaminophenol in one-step method, through the assistance of ultrasonic waves, using a solid superbasic catalyst system, to overcome the use of expensive m-aminophenol in the traditional
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Embodiment 1
[0024] Embodiment 1. The preparation of super base catalyst:
[0025] Make 10g of potassium hydroxide into a 5% solution, add 90g of magnesium oxide, stir evenly, dry, and calcinate at 700~800°C for 2 hours under the protection of nitrogen to obtain a super-strong base catalyst, which is sealed and stored for later use.
[0027] In a 500ml flask, add 200g of diethylamine, 10g of catalyst sodium amide and 5g of super base catalyst, stir and cool down to 5°C, dropwise add 15g of o-chlorophenol and complete the dropwise addition within 15 minutes. Turn on the ultrasonic wave, the ultrasonic frequency is 40kHz, the ultrasonic power is 100w, the temperature is raised to the reflux state of diethylamine, and the reaction is completed for 20 minutes. Recover diethylamine by rotary evaporation, add 60g of toluene, drop the temperature below 5°C and drop 75g of water to quench the reaction, add dropwise 5% hydrochloric acid aqueous solution to adjust pH=7, separate liquid, wash with water, separate liquid, rotary steam organic phase to obtain the product m-diethylaminophenol 18.9g, yield 98.5%, purity 99.1%.
[0029] In a 500ml flask, add 200g of diethylamine, add 10g of catalyst sodium amide, 5g of super base catalyst, stir and lower the temperature to 5°C, dropwise add 15g of o-chlorophenol and complete the dropwise addition within 15 minutes. Turn on the ultrasonic wave, the ultrasonic frequency is 30kHz, the ultrasonic power is 100w, the temperature is raised to the reflux state of diethylamine, and the reaction is completed for 15 minutes. Recover diethylamine by rotary evaporation, add 60g of toluene, drop the temperature below 5°C and drop 75g of water to quench the reaction, add dropwise 5% hydrochloric acid aqueous solution to adjust pH=7, separate liquid, wash with water, separate liquid, rotary steam organic phase to obtain the product m-diethylaminophenol 18.8g, yield 97.8%, purity 99.2%.
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Abstract
The invention provides a method for synthesizing m-diethylaminophenol. The method comprises the following steps: mixing potassium hydroxide and magnesium oxide, and calcining at 700-800 DEG C to obtain a solid super base catalyst; adding sodium amide and the solid super base catalyst into diethylamine, stirring, keeping the temperature at 3-8 DEG C, dropwise adding o-chlorophenol within 20 minutes, stirring for 10-20 minutes after dropwise adding is finished, starting ultrasonic oscillation, heating, carrying out reflux reaction for 10-30 minutes, carrying out reduced pressure rotary evaporation to recover diethylamine, adding xylene, stirring, cooling to 5 DEG C or below, and adding water to quench the catalyst; and adjusting the pH value of a water layer to be neutral or weakly acidic, and recovering xylene to obtain the m-diethylaminophenol finished product. The method disclosed by the invention not only is short in time and high in efficiency, but also does not use expensive m-aminophenol raw materials, so that the problem of troublesome post-treatment is solved; meanwhile, potential safety hazards caused by using unsafe catalysts can be avoided, so that m-diethylaminophenol production is safer, more economical and more efficient, and industrialization is better facilitated.
Description
technical field [0001] The invention relates to a method for synthesizing an intermediate compound, in particular to a method for synthesizing m-diethylaminophenol. Background technique [0002] m-diethylaminophenol, English name: m-diethy aminophenol, properties: white crystal; color darkens when exposed to light and air. The melting point is 78°C. The boiling point is 276-280°C. Insoluble in water. m-diethylaminophenol is used in the manufacture of xanthone dyes, etc., is a dye intermediate, used in dyes, medicine, cosmetics, etc., is used in the production of acid rose red B, cationic brilliant yellow 10GFF, cationic emerald blue GB, acid medium pink 3M, basic rhodamine B, basic rhodamine and other important raw materials. [0003] With the more and more widespread use of heat and pressure sensitive dyes, m-diethylaminophenol has received more and more attention. At present, the main synthetic route of m-diethylaminophenol in China is to reduce sodium m-nitrobenzenes...
Claims
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