Method for synthesizing o-nitrophenylacetic acid

A synthesis method and technology of o-nitrobenzene are applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problems of difficulty in obtaining, high cost, pollution and the like, Achieve the effect of improving yield, shortening reaction time, and strengthening separation effect

Inactive Publication Date: 2018-11-06
杨程飞扬
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The classic synthetic method of o-nitrophenylacetic acid is not easy to obtain because the raw material o-nitrophenylacetonitrile, and the traditional process of synthesizing o-nitrophenylacetonitrile requires the use of sodium cyanide, a relatively toxic substance and serious pollution, so it cannot be used Adapt to the current industrial production requirements
Due to the relative excess of o-nitrotoluene production, a relatively cheap and environmentally friendly method for the synthesis of o-nitrophenylacetic acid using o-nitrotoluene as a raw material is studied to improve the problems of low yield, high cost and poor safety

Method used

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  • Method for synthesizing o-nitrophenylacetic acid

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Embodiment 1

[0018] 1, a kind of synthetic method of intermediate o-nitrophenylacetic acid, it is characterized in that the method comprises the following steps:

[0019] Step 1. Add 100ml of absolute ethanol into a 500ml four-necked flask equipped with a thermometer, and gradually add 0.1g of catalyst Pt-MgO-CNTs and 8g of sodium metal while stirring;

[0020] Step 2. After the reaction is completed, when the temperature drops to room temperature, add 35ml o-nitrotoluene and 56ml diethyl oxalate, heat to 45°C for 3 hours, then add water and heat up to 60°C for hydrolysis reaction;

[0021] Step 3. After reacting for 1 hour, lower the temperature to 35° C. and carry out vacuum distillation until the distilled components are cloudy liquids. will reverse

[0022] Cool the solution to 10°C and adjust the pH to 7 with sodium hydroxide solution;

[0023] Step 4, then dropwise add hydrogen peroxide solution with a concentration of 0.3M, control its dropping speed, keep the temperature below 20...

Embodiment 2

[0031] Step 2. After the reaction is completed, when the temperature drops to room temperature, add 30ml of o-nitrotoluene and 56ml of diethyl oxalate, heat to 45°C for 3 hours, then add water and heat up to 60°C for hydrolysis reaction; the rest of the steps are the same as in Example 1 .

Embodiment 3

[0033] Step 2. After the reaction is completed, when the temperature drops to room temperature, add 25ml o-nitrotoluene and 56ml diethyl oxalate, heat to 45°C for 3 hours, then add water and heat up to 60°C for hydrolysis reaction; the rest of the steps are the same as in Example 1 .

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Abstract

The invention discloses a method for synthesizing o-nitrophenylacetic acid. Absolute ethyl alcohol, Pt-MgO-CNTs, metal sodium, o-nitrotoluene, diethyl oxalate, hydrogen peroxide and H2PtCl6 are used as main raw materials, the synthesis process adopts the o-nitrotoluene and diethyl oxalate to be subjected to condensation reaction to obtain the o-nitrophenylacetic acid under the action of the catalyst Pt-MgO-CNTs, the separation method of steam distillation is replaced by vacuum distillation, the reaction time is greatly shortened, and the separation effect is significantly enhanced. The optimummaterial ratio, the temperature of oxidation reactions and the temperature and time of condensation reactions are optimized by a large number of experiments, and the yield is greatly improved.

Description

technical field [0001] The invention relates to a method for synthesizing o-nitrophenylacetic acid, which belongs to the field of chemical synthesis. Background technique [0002] 2-Nitrophenylacetic acid (2-Nitrophenylacetic acid) CAS: 3740-52-1 is a widely used intermediate in organic synthesis. O-nitrophenylacetic acid can be used to synthesize benzofuran-2(3H)-one through ammonium sulfide reduction, diazotization reaction, and hydrolysis. Benzofuran-2(3H)-one is an important organic synthesis intermediate that can be used in Synthetic medicines, pesticides and new antioxidants. The classic synthetic method of o-nitrophenylacetic acid is not easy to obtain because the raw material o-nitrophenylacetonitrile, and the traditional process of synthesizing o-nitrophenylacetonitrile requires the use of sodium cyanide, a relatively toxic substance and serious pollution, so it cannot be used Adapt to the current industrial production requirements. Due to the relative excess of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C201/16C07C205/56B01J23/42
CPCB01J23/42C07C201/12C07C201/16C07C205/56
Inventor 杨程飞扬冯杰
Owner 杨程飞扬
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