Method for synthesizing anisyl methyl ketone

A methoxyacetophenone and methoxylation technology, applied in the chemical industry, can solve the problems of high regeneration temperature of HZSM-5 molecular sieve, high experimental cost, low recovery rate, etc., and achieve good promotion value and high experimental yield. , the effect of less by-products

Inactive Publication Date: 2008-09-24
BAOSHAN IRON & STEEL CO LTD
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Problems solved by technology

The regeneration temperature of HZSM-5 molecular sieve used in this meth

Method used

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  • Method for synthesizing anisyl methyl ketone
  • Method for synthesizing anisyl methyl ketone
  • Method for synthesizing anisyl methyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Put 47.05g of phenol, 100g of acetonitrile and 80g of 35% hydrochloric acid into a 250ml four-neck flask, heat to 100°C, and observe the changes of reactants and products. After reacting for 2h to the end point, neutralize, cool and crystallize, filter and dry.

[0041] Put 50g of the above-mentioned crystals, 150g of toluene and 20g of methanesulfonic acid into a 250ml four-neck flask, heat to 90°C, and react for 2.5h. Cool to 20°C, crystallize, filter, and dry to obtain coarse crystals, and the filtrate is recycled.

[0042] The crude crystals were recrystallized at a recrystallization temperature of 108° C., filtered, and dried to obtain p-acetylphenol with a purity of 98.6%.

[0043] Take 30g of p-acetylphenol, dissolve it in aqueous sodium hydroxide solution, adjust the pH to about 10, and the temperature is 45°C, slowly add 32g of dimethyl sulfate, and react for 2.5h to obtain 28.8g of colorless crystals with strong fragrance, melting point 37.4-38.6°C.

[0044...

Embodiment 2

[0046] Put 45g of phenol, 95g of acetonitrile and 75g of 40% sulfuric acid into a 250ml four-neck flask, heat to 96°C, and observe the changes of reactants and products. Reaction 1.5h. Neutralize, cool and crystallize, filter and dry.

[0047] Put 46g of the above-mentioned crystals, 150g of toluene and 20g of methanesulfonic acid into a 250ml four-neck flask, heat to 88°C, and react for 2h. Cool to 20°C, crystallize, filter, and dry to obtain coarse crystals, and the filtrate is recycled.

[0048] The crude crystals were recrystallized at a recrystallization temperature of 109° C., filtered, and dried to obtain p-acetylphenol with a purity of 99.2%.

[0049]Take 28g of p-acetylphenol, dissolve it in aqueous sodium hydroxide solution, adjust the pH to about 11, and the temperature at 42°C, and slowly add 31g of dimethyl sulfate. After reacting for 3 hours, 27.6 g of colorless crystals with a strong aroma were obtained, with a melting point of 37.7-38.6°C.

[0050] The melt...

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Abstract

The present invention provides a method used for synthesizing p methoxyacetophenone with phenol. The method comprises the following steps: an acylating agent and the phenol react to prepare phenyl acetate with a catalyst; the phenyl acetate is recomposed and separated to prepare acetyl phenol; the acetyl phenol is used for preparing the p methoxyacetophenone through methoxylation. Compared with the traditional synthetic method of the p methoxyacetophenone, the method has the characteristics of low price in producing the raw materials, mild experimental conditions, less by-products in the experiment and high yield of the product.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for synthesizing p-methoxyacetophenone, more specifically to a method for synthesizing p-methoxyacetophenone with phenol as a raw material. Background technique [0002] p-Methoxyacetophenone is mainly used in the production of flavors and fragrances, pharmaceuticals, and cosmetic intermediates. For example, p-methoxyphenylacetic acid can be prepared from p-methoxyacetophenone, which is used as an intermediate for puerarin. Puerarin is an important medical raw material. At present, there is no artificially synthesized puerarin in China. P-methoxyacetophenone and can be used in the production of liquid crystal monomers. In the synthesis of high-grade acetylenic liquid crystals, there is a process that uses p-methoxyacetophenone as the initial synthetic raw material, which is still in the research and development stage in China) is a relatively promising fine chemical pr...

Claims

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Application Information

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IPC IPC(8): C07C49/84C07C45/54
Inventor 刘春法孙剑
Owner BAOSHAN IRON & STEEL CO LTD
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