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Production process of p-hydroxyacetophenone

A technology for p-hydroxyacetophenone and production process, which is applied in the field of production technology of p-hydroxyacetophenone, can solve the problems of difficult separation of homogeneous catalysts, low reaction selectivity and high processing cost, and achieves improvement of reaction degree and reaction efficiency , enhance nucleophilicity, accelerate the effect of forming reaction

Pending Publication Date: 2020-11-03
湖北顺明化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When these catalysts are used, the reaction conversion rate is high and the reaction time is short, but these catalysts will produce more by-products in the reaction process, making the reaction selectivity lower, and it is very difficult to separate them from the reaction system as a homogeneous catalyst. Difficult, high processing cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A production technique for p-hydroxyacetophenone, comprising the following steps:

[0028] Step S1: water-phase esterification: first dissolve 600 kg of measured phenol in 1000 kg of potassium hydroxide solution to form a prefabricated liquid, pump the prefabricated liquid and 20 kg of 2-mercapto-R-butyrolactone into the reaction kettle, and then Pump 715kg of acetic anhydride liquid, stir and react in a stirring environment at room temperature 25°C for 8 hours, the reaction of the central control phenol is complete, and the acetic acid and excess acetic anhydride are distilled off under reduced pressure after completion, to obtain a dark red intermediate phenyl acetate liquid;

[0029] Step S2: Rearrangement synthesis reaction: use a metering pump to pump 800 kg of o-dichlorobenzene into the rearrangement kettle, put in 200 kg of anhydrous aluminum trichloride, 20 kg of cetearyl alcohol and trimethylsiloxyphenyl polydimethylsiloxane Base siloxane 10kg, micro-negative p...

Embodiment 2

[0034] A production technique for p-hydroxyacetophenone, comprising the following steps:

[0035] Step S1: Aqueous phase esterification: first dissolve 600kg of measured phenol in 1000kg of ammonia solution to form a prefabricated solution, pump the prefabricated solution and 40kg of 2-mercapto-R-butyrolactone into the reaction kettle with a metering pump, and then pump into 715kg of acetic anhydride liquid, stirred and reacted in a stirring environment at room temperature 25-30°C for 8-10 hours, the reaction of the central control phenol was complete, and the acetic acid and excess acetic anhydride were distilled under reduced pressure to obtain a dark red intermediate phenyl acetate liquid;

[0036] Step S2: Rearrangement synthesis reaction: Use a metering pump to pump 800-1000 kg of o-dichlorobenzene into the rearrangement kettle, put in 200 kg of anhydrous aluminum trichloride, 30 kg of cetearyl alcohol and trimethylsiloxyphenyl poly 20kg of dimethylsiloxane, micro-negativ...

Embodiment 3

[0041] A production technique for p-hydroxyacetophenone, comprising the following steps:

[0042] Step S1: water-phase esterification: first dissolve 600 kg of measured phenol in 1000 kg of sodium hydroxide solution to form a prefabricated liquid, pump the prefabricated liquid and 30 kg of 2-mercapto-R-butyrolactone into the reaction kettle, and then Pump in 715kg of acetic anhydride liquid, stir and react for 8-10 hours in a stirring environment at room temperature 25-30°C, the reaction of the central control phenol is complete, and the acetic acid and excess acetic anhydride are distilled off under reduced pressure to obtain a dark red intermediate phenyl acetate liquid ;

[0043]Step S2: rearrangement synthesis reaction: use a metering pump to pump 900 kg of o-dichlorobenzene into the rearrangement kettle, put in 200 kg of anhydrous aluminum trichloride, 25 kg of cetearyl alcohol and trimethylsiloxyphenyl polydimethylsiloxane Base siloxane 15kg, micro-negative pressure is ...

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Abstract

The invention provides a production process of p-hydroxyacetophenone, which comprises the following steps: S1: water-phase esterification: dissolving phenol in an alkaline solution to form a prefabricated solution, adding the prefabricated solution and 2-mercapto-R-butyrolactone into a reaction kettle, adding acetic anhydride, and carrying out stirring reaction at normal temperature for 8-10 hours; s2, rearrangement synthesis reaction: adding o-dichlorobenzene and a catalyst into the reaction kettle, stirring and heating to 90-100 DEG C, slowly dropwise adding phenyl acetate into the reactionkettle, and keeping the temperature for 2-3 hours; s3, cooling and separating the reaction product; step S4, layering and recovering the reaction product; S5, rectification: feeding the reaction product into a rectifying tower to recover hydroxyacetophenone and o-hydroxyacetophenone, wherein the catalyst is prepared from the following components in parts by weight: 100 parts of anhydrous aluminumtrichloride and 10-15 parts of cetostearyl alcohol. The production process of p-hydroxyacetophenone has the advantages of high reaction conversion rate, high reaction efficiency, fewer byproducts generated in the catalytic reaction of the catalyst and high selectivity of the catalytic reaction.

Description

technical field [0001] The invention relates to the technical field of production of pharmaceutical intermediates, in particular to a production process of p-hydroxyacetophenone. Background technique [0002] p-Hydroxyacetophenone (p-Hydroxyacetophenone, abbreviated as p-HAP), commonly known as abietol, the molecular formula is C 8 h 8 o 2 . It naturally exists in the stems, leaves, fungi and roots of some plants of the family Asteraceae. In industry, it is mainly obtained from phenol as raw material through acylation and Fries rearrangement. p-Hydroxyacetophenone is mainly used in medicine, spices and other industrial fields, and its downstream products include atenolol, N-acetyl para-aminophenol, 4-hydroxystyrene and so on. [0003] In the traditional synthetic process route of p-hydroxyacetophenone, the reaction is divided into two steps. The first step is to synthesize phenyl acetate from phenol and acetic anhydride. ethyl ketone. The catalysts used in these two s...

Claims

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Application Information

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IPC IPC(8): C07C45/54C07C49/825C07C67/08C07C69/157
CPCC07C67/08C07C45/54C07C69/157C07C49/825
Inventor 朱从东雷药安桑兵
Owner 湖北顺明化工有限公司
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