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A kind of preparation method of phenyl acetate compound

A technology of phenyl acetate and compounds, which is applied in the field of preparation of phenyl acetate compounds, can solve the problems of expensive acidic catalysts, difficult nitrogen-containing wastewater treatment, large amount of alkaline reagents, etc., and achieves easy automatic control and heat transfer effects Poor, fast heat transfer effect

Active Publication Date: 2022-02-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1) The amount of alkaline reagents is large, the treatment of nitrogen-containing wastewater is difficult, the post-treatment is troublesome, and the amount of three wastes is large, which is not conducive to environmental protection;
[0005] 2) Acidic catalysts are expensive, high cost, harsh reaction conditions and long reaction time
[0006] 3) Due to the large amount of materials in the batch (kettle) reaction, active reagents such as acetic anhydride and acetyl chloride used in the reaction are easily decomposed when exposed to water and air, and are easy to flush or even explode, posing a great safety hazard

Method used

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  • A kind of preparation method of phenyl acetate compound
  • A kind of preparation method of phenyl acetate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add deionized water (30 L), phenol (9.4kg, 100mol) and sodium hydroxide (4.4kg, 110mol) to the first storage tank A in sequence and stir to dissolve until clear, then add deionized water to accurately make up to 50 L to make an aqueous solution with a phenol concentration of 2.0 mol / L, stir evenly and seal it for use. Add 13.3 kg of acetic anhydride (130 mol, density 1.08 g / mL, molar concentration 10.60 mol / L) into the second storage tank B and seal it for use.

[0023] The materials in the first storage tank A and the second storage tank B are transported to the mixer T through the first metering pump P1 and the second metering pump P2 respectively for mixing (the molar flow ratio of phenol: acetic anhydride is controlled to be 1:1.3 ), the mixed solution continuously enters the tubular reactor R for esterification reaction, the temperature inside the tubular reactor R is maintained at 20°C, and the residence time of the mixed solution in the tubular reactor R is 2 min...

Embodiment 2

[0025] In the first storage tank A, add deionized water (30 L), p-cresol (10.8kg, 100mol), sodium hydroxide (4.4kg, 110mol) and stir until clear, then add deionized water Determine the volume to 50 L, make an aqueous solution with a p-cresol concentration of 2.0 mol / L, stir well and seal it for use. Add 13.3 kg of acetic anhydride (130 mol, density 1.08 g / mL, molar concentration 10.60 mol / L) into the second storage tank B and seal it for use.

[0026] Use a metering pump to transport the materials in the first storage tank A and the second storage tank B to the mixer for mixing (control the molar flow ratio of p-cresol: acetic anhydride to be 1:1.3), and the mixed solution enters continuously The esterification reaction was carried out in the tubular reactor, the temperature inside the tubular reactor was maintained at 20° C., and the residence time of the mixed solution in the tubular reactor was 2 minutes. The feed liquid after the esterification reaction flowing out of the...

Embodiment 3

[0028] Add deionized water (30 L), p-nitrophenol (13.9kg, 100mol) and sodium hydroxide (4.4kg, 110mol) to the first storage tank A in sequence and stir until clear, then add deionized water Determine the volume to 50 L, make an aqueous solution with a p-nitrophenol concentration of 2.0 mol / L, stir well and seal it for use. Add 13.3 kg of acetic anhydride (130 mol, density 1.08 g / mL, molar concentration 10.60 mol / L) into the second storage tank B and seal it for use.

[0029] Use a metering pump to transport the materials in the first storage tank A and the second storage tank B to the mixer for mixing (control the molar flow ratio of p-nitrophenol: acetic anhydride to be 1:1.3), and the mixed solution enters continuously The esterification reaction was carried out in the tubular reactor, the temperature inside the tubular reactor was maintained at 20° C., and the residence time of the mixed solution in the tubular reactor was 2 minutes. The feed liquid after the esterificatio...

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Abstract

The invention discloses a method for preparing phenyl acetate compounds. It uses substituted phenol and acetic anhydride as shown in the formula (I) as reaction raw materials, and uses aqueous sodium hydroxide solution as a solvent to perform esterification in a tubular reactor. reaction to obtain phenyl acetate compounds shown in formula (II), the reaction formula is as follows: in formula (I) and formula (II), the substituent R is hydrogen, C1-C6 alkyl, nitro, A cyano group, a halogen group, a carboxyl group or a C1-C12 alkoxycarbonyl group. The invention adopts a tubular reaction approaching plug flow, in which there is almost no back-mixing of materials, high mass and heat transfer efficiency, significantly reduced occurrence of side reactions, and high product yield and purity.

Description

technical field [0001] The invention relates to a preparation method of phenyl acetate compounds. Background technique [0002] Substituted phenyl acetate series compounds are important intermediates, which are widely used in the fields of medicine, chemical industry, pesticides, etc. For example, phenyl acetate can be used to synthesize choleretic drug p-hydroxyacetophenone, and p-nitrophenyl acetate is a β-receptor It is an important raw material of the body blocker celiprolol hydrochloride, and acetylsalicylic acid can be used as an antipyretic and analgesic. [0003] At present, the main method of synthesizing phenyl acetate series compounds is to use phenol as a raw material, and undergo an esterification reaction under the action of a base such as pyridine (Heter°Cyclic Communications, 2017, 23(4), 325-330330; Org. Lett.2014, 16 , 236−239), and esterification can also occur under Lewis acid catalysis (Tetrahedron Letters, 2014,55(4), 910-912; Heter℃yclic Letters, 6(2)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/157C07C201/12C07C205/43
CPCC07C67/08C07C201/12
Inventor 金灿孙彬苏为科
Owner ZHEJIANG UNIV OF TECH
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