Synthesis method of 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, poor safety, etc. , to achieve the effect of strengthening the separation effect, shortening the reaction time and improving the yield

Inactive Publication Date: 2018-12-14
XUZHOU NORMAL UNIVERSITY
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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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  • Synthesis method of O-nitrophenylacetic acid

Examples

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Comparison scheme
Effect test

Embodiment 1

[0018] A kind of synthetic method of intermediate o-nitrophenylacetic acid 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°C, and...

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 synthesis method of O-nitrophenylacetic acid; anhydrous ethanol, Pt-MgO-CNTs, metallic sodium, O-nitrotoluene, diethyl oxalate, hydrogen peroxide and H2PtCl6 are used as mainraw materials; according to the synthesis process, O-nitrotoluene and diethyl oxalate are subjected to condensation reaction under the action of the catalyst Pt-MgO-CNTs to obtain O-nitrophenylaceticacid; reduced pressure distillation replaces a separation method of water steam distillation, so the reaction time is greatly shortened and the separation effect is enhanced obviously. The optimum material ratio, oxidation reaction temperature and condensation reaction temperature and time are optimized through 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): C07C205/56C07C201/12B01J23/58
CPCB01J23/58C07C201/12C07C205/56
Inventor 邵亚陈浩
Owner XUZHOU NORMAL UNIVERSITY
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