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Method for preparing m-nitrophenol ester by solid-phase reaction system

A technology of nitrophenol ester and solid phase reaction, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex preparation methods, high toxicity of acetonitrile, high price, etc., and achieve simple post-processing, The effect of less toxic side effects and short reaction time

Inactive Publication Date: 2018-08-03
ZHEJIANG UNIV
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Problems solved by technology

[0003] Using acetic anhydride and m-nitrophenol as raw materials to prepare m-nitrophenol ethyl ester requires catalyst SBA-15–Ph–Pr–SO3H to catalyze the reaction; SBA-15–Ph–Pr–SO3H is a hydrophobic sulfonic acid , the price is more expensive, and the preparation method is more complicated
[0004] Utilize acetyl chloride and m-nitrophenol to prepare m-nitrophenol ethyl ester and need to utilize ZrOCl 2 .8H 2 O is a catalyst, carried out in acetonitrile solvent, acetonitrile is highly toxic

Method used

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  • Method for preparing m-nitrophenol ester by solid-phase reaction system
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  • Method for preparing m-nitrophenol ester by solid-phase reaction system

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Embodiment 1

[0021] Embodiment 1, a kind of preparation method of ethyl m-nitrophenolate, take m-dinitrobenzene and sodium acetate as raw material, carry out the following steps successively:

[0022] 1) Take 16.8g (0.1mol) of m-dinitrobenzene and 8.2g (0.1mol) of sodium acetate, put them in a 50mL stainless steel screw cap grinding jar, seal it and fix it on the Mixer Mill 400 mixing mill , set the vibration frequency to 30 Hz, and grind at 10°C for 20 min.

[0023] 2), wash with 150mL of anhydrous methanol after the reaction, filter, repeat 3 times, combine the filtrate, reduce pressure (vacuum degree is 40mmHg) after distilling methanol in the filtrate, column chromatography separates the product;

[0024] The column chromatography is as follows: 20-50 g of 200-300-mesh column chromatography silica gel is installed in the glass chromatography column, and all the filtrate after distilling methanol is loaded, and ethyl acetate:petroleum ether=1:2 The mixed solution of (volume ratio) is a...

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Abstract

The invention discloses a method for preparing m-nitrophenol ester by a solid-phase reaction system. According to the invention, m-dinitrobenzene and carboxylate are taken as raw materials, the methodcomprises the following steps: 1) m-dinitrobenzene and carboxylate are mixed and ground at the temperature of 10-80 DEG C for 20-180 min; wherein the mol ratio of m-dinitrobenzene to carboxylate 1:1-1:5; and 2) the ground material is washed with absolute methanol and then filtered, after steaming methanol of a filtrate, through column chromatography separating, ethyl acetate / petroleum ether is taken as an eluant for separation by passing a column, and an eluant is subjected to pressure reduction steaming to obtain the m-nitrophenol ester. The m-nitrophenol ester has the advantages of concisetechnology, no solvent, short reaction time, mild condition, high yield, and good selectivity.

Description

technical field [0001] The invention belongs to the synthesis reaction of an organic compound in a solid-phase reaction system, and relates to a preparation method of an organic compound m-nitrophenol ester. Background technique [0002] Ethyl m-nitrophenolate with the structural formula shown in Formula 1 is a chemical synthesis intermediate. The main synthetic route of m-nitrophenol ethyl ester is, by m-nitrophenol as raw material, with acetic anhydride (Can.J.Chem.2012,90,464-468) or acetyl chloride (Tetrahedron Letters 2005,46,147- 151) prepared by reaction. [0003] Using acetic anhydride and m-nitrophenol as raw materials to prepare m-nitrophenol ethyl ester requires catalyst SBA-15–Ph–Pr–SO3H to catalyze the reaction; SBA-15–Ph–Pr–SO3H is a hydrophobic sulfonic acid , the price is more expensive, and the preparation method is more complicated. [0004] Utilize acetyl chloride and m-nitrophenol to prepare m-nitrophenol ethyl ester and need to utilize ZrOCl 2 .8H 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/43
CPCC07C201/12C07C205/43
Inventor 陈新志卢芊芊高锐钱超
Owner ZHEJIANG UNIV
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