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A kind of preparation and crystallization method of phenacetin

A phenacetin and crystallization technology, which is applied in the preparation of organic compounds, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve the problems of expensive bromide high-risk operation, long synthesis cycle, poor product quality, etc. Batch production cycle, short reaction time, good stability

Active Publication Date: 2017-11-07
济南鼎皓医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0034] In order to make up for the above deficiencies and overcome the defects of cumbersome process, poor product quality, low yield, long synthesis cycle, expensive bromide and high-risk operation, the present invention provides a method for the preparation and crystallization of phenacetin

Method used

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  • A kind of preparation and crystallization method of phenacetin
  • A kind of preparation and crystallization method of phenacetin
  • A kind of preparation and crystallization method of phenacetin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The preparation and crystallization method of phenacetin comprises steps:

[0057] 1) Preparation of p-ethoxyaniline sulfate

[0058] Pump 210L of purified water into a 500L reactor, add 20.6kg of p-ethoxyaniline, control the temperature at 15-20°C, add 16.1kg of sulfuric acid, control the temperature at 15-20°C, and stir for 1 hour to obtain clarified p-ethoxyaniline Aniline Sulfate Sulfate Solution.

[0059] 2) Preparation of phenacetin

[0060] Heat up the p-ethoxyaniline sulfate solution, control the temperature at 95~100°C, add 17.6kg of acetic anhydride dropwise, add potassium acetate buffer salt to control the pH4~5, control the temperature at 95~100°C and stir for 6 hours, the reaction is over , lowered the temperature to 50°C, slowly added a mixture of 35 L of water and 105 L of isopropanol, stirred at room temperature for 1 hour, and centrifuged and dried to obtain 25.6 kg of crystalline phenacetin with a yield of 95.0% and a purity of 99.3%.

[0061] The l...

Embodiment 2

[0063] The preparation and crystallization method of phenacetin comprises steps:

[0064] 1) Preparation of p-ethoxyaniline phosphate

[0065] Pump 225L of purified water into a 500L reactor, add 20.6kg of p-ethoxyaniline, control the temperature at 15-20°C, add 16.3kg of phosphoric acid, control the temperature at 15-20°C, and stir for 1 hour to obtain clarified p-ethoxyaniline aniline phosphate solution.

[0066] 2) Preparation of phenacetin

[0067] Heat up the p-ethoxyaniline phosphate solution, control the temperature at 95~100°C, add 17.6kg of acetic anhydride dropwise, add ammonium acetate buffer salt to control the pH4~5, control the temperature at 95~100°C and stir for 6 hours, the reaction is over , lowered the temperature to 50°C, slowly added a mixture of 35 L of water and 105 L of isopropanol, stirred at room temperature for 1 hour, and centrifuged and dried to obtain 25.7 kg of crystalline phenacetin with a yield of 95.5% and a purity of 99.2%.

Embodiment 3

[0069] The preparation and crystallization method of phenacetin comprises steps:

[0070] 1) Preparation of bromide salt of p-ethoxyaniline

[0071] Pump 180L of purified water into a 500L reactor, add 20.6kg of p-ethoxyaniline, control the temperature at 30-35°C, add 24.3kg of hydrobromic acid, control the temperature at 30-35°C, and stir for 40 minutes to obtain clarified paraben Oxyaniline bromide salt solution.

[0072] 2) Preparation of phenacetin

[0073] Heat up the p-ethoxyaniline phosphate solution, control the temperature at 90~93°C, add 18.52kg of acetic anhydride dropwise, add calcium acetate buffer salt to control the pH4~5, control the temperature at 90~93°C and stir for 6.5 hours, the reaction is over , lowered the temperature to 45°C, slowly added a mixture of 30L of water and 120L of ethanol, stirred at room temperature for 1 hour, and centrifuged and dried to obtain 25.5kg of crystalline phenacetin, with a yield of 94.7% and a purity of 99.1%.

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Abstract

The invention discloses a preparation and crystallization method of phenacetin, and belongs to the field of chemical industry. According to the preparation and crystallization method, p-phenetidine is reacted with an acid in water so as to obtain a p-phenetidine salt; the p-phenetidine salt is reacted with an anhydride in a buffer solution system; after reaction, a mixed solution of water and an organic solvent is added into an obtained reaction solution, and phenacetin crystals are obtained via stirring. Product yield is high; two-step reaction total yield is higher than 92%; the obtained products are crystalline solids; stability is high; purity is high, and is higher than 99%; reaction time is short; reaction conditions are mild; product separation operation is simple; direct filtering separation can be carried out after reaction; and batch production period is shortened greatly.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation and crystallization method of phenacetin. Background technique [0002] The structural formula of phenacetin is: [0003] [0004] Phenacetin was first synthesized by Morse in 1878 and listed in the United States in 1887. It is the first synthetic antipyretic and analgesic drug on the market. It is often used to treat headache, fever, neuralgia, etc. Phenacetin is mainly used for compatibility with aspirin and caffeine to make a compound preparation APC for antipyretic and analgesic treatment of colds. The antipyretic and analgesic effect of phenacetin is similar to that of "acetylsalicylic acid". It is mainly used as an antipyretic and analgesic drug with slow and long-lasting effect. It has good curative effect on the treatment of headache, neuralgia, joint pain and fever. , but the anti-rheumatic and anti-inflammatory effects are weak. Phenacetin is also an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/25C07C231/02C07C231/24
Inventor 陈志桥陈成文方金印颜猛
Owner 济南鼎皓医药科技有限公司
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