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Salicylamide synthesis method

A technology of salicylamide and synthesis method, which is applied in the field of salicylamide preparation, can solve the problems of long process flow, high production cost and high energy consumption

Inactive Publication Date: 2019-08-30
ZHENJIANG GAOPENG PHARMA
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Problems solved by technology

[0002] Salicylamide is a widely used fine chemical intermediate, which can be used to synthesize organic chemicals such as nifesamide and o-ethoxy formamide, and is also commonly used in the fields of medical treatment, spices, fuels and rubber additives. Salicylamide is a kind of antipyretic analgesic used in large quantities, can be used for treating fever headache, neuralgia, arthralgia and rheumatic arthralgia etc., at present, the method for synthesizing salicylamide mainly is salicylic acid ammoniation method and Methyl salicylate ammonification method, these two synthesis methods have long process flow, large equipment investment, high energy consumption, high production cost, and produce a large amount of acid-base waste liquid at the same time, polluting the environment

Method used

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preparation example Construction

[0017] A method for synthesizing salicylamide, using urea and phenol as raw materials not only realizes the comprehensive utilization of urea, but also promotes the clean production of salicylamide. By mixing zinc oxide and calcium oxide with higher catalytic activity, the yield of salicylamide is improved. Synthetic efficiency, the catalytic mode and mechanism of zinc oxide and calcium oxide are different, zinc oxide is a homogeneous catalyst precursor for the reaction of urea and phenol to synthesize salicylamide, while calcium oxide is a heterogeneous catalyst for the reaction, and the mixture of zinc oxide and calcium oxide has The role of synergistic catalysis mainly includes the following steps:

[0018] Step 1: preparing catalyst A, baking calcium carbonate at 780-800°C for 5-6 hours in a nitrogen-sealed environment to obtain calcium oxide;

[0019] Step 2: preparing catalyst B, calcining zinc oxide at 400-500° C. for 1-2 hours in a nitrogen-tight environment to obtain ...

Embodiment 1

[0028] Add 6g of urea and 94g of phenol into a high-pressure reactor with magnetic stirring, and heat up to 250°C for 12 hours under magnetic stirring. After the reaction, cool the reactor to room temperature, take out the liquid product, separate and mix The catalyst is used to obtain a salicylamide solution, and the salicylamide solution can be dried to obtain salicylamide. The drying temperature is 120° C., the drying time is 45 minutes, and the yield of salicylamide is 4.1%.

Embodiment 2

[0030] Add 6g of urea, 94g of phenol, and 0.2g of catalyst A into a high-pressure reactor with magnetic stirring. Under magnetic stirring, heat up to 230°C to react for 12 hours. After the reaction, cool the reactor to room temperature and take it out. Liquid product, separate mixed catalyst to obtain salicylamide solution, salicylamide solution can be dried to obtain salicylamide, the drying temperature is 120°C, the drying time is 45 minutes, and the yield of salicylamide is 19.3%;

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Abstract

The invention provides a salicylamide synthesis method. The salicylamide synthesis method mainly comprises the following steps: step 1, preparing a catalyst A; step 2, preparing a catalyst B; step 3,preparing a mixed catalyst; step 4, reacting; step 5, drying; and step 6, recovering the catalyst. By using urea and phenol as raw materials, comprehensive utilization of the urea can be realized, meanwhile, clean production of salicylamide can be promoted, zinc oxide and calcium oxide which are high in catalytic activity are mixed to improve the synthesis efficiency of the salicylamide, catalyticmodes and mechanisms of the zinc oxide and the calcium oxide are different, the zinc oxide is a homogeneous catalyst precursor for the reaction of the urea and the phenol to synthesize the salicylamide, but the calcium oxide is a heterogeneous catalyst for the reaction, and the mixture of the zinc oxide and the calcium oxide has a synergistic catalytic effect.

Description

technical field [0001] The invention relates to the technical field of preparation of salicylamide, in particular to a method for synthesizing salicylamide. Background technique [0002] Salicylamide is a widely used fine chemical intermediate, which can be used to synthesize organic chemicals such as nifesamide and o-ethoxy formamide, and is also commonly used in the fields of medical treatment, spices, fuels and rubber additives. Salicylamide is a kind of antipyretic analgesic used in large quantities, can be used for treating fever headache, neuralgia, arthralgia and rheumatic arthralgia etc., at present, the method for synthesizing salicylamide mainly is salicylic acid ammoniation method and Methyl salicylate ammonification method, these two synthesis methods have long process flow, large equipment investment, high energy consumption, high production cost, and produce a large amount of acid-base waste liquid at the same time, polluting the environment. Contents of the ...

Claims

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Application Information

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IPC IPC(8): C07C231/10C07C235/60B01J23/06
CPCC07C231/10B01J23/06B01J23/02B01J35/19C07C235/60
Inventor 王成慧王成栋李冕
Owner ZHENJIANG GAOPENG PHARMA
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