Synthesis process method and device of 4-acetophenetidine bulk drug

A technology for p-aminophenethyl ether and acetaminophen, which is applied in the field of raw material drug production, can solve problems such as complicated processes, limited raw materials, etc., and achieve the effects of easy availability of raw materials, novel overall structure, and convenient actual production and use.

Pending Publication Date: 2020-04-10
李宾
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the deficiencies in the prior art, solve the complex and complex process of the existing p-acetamidophenetole, the raw materials used are limited

Method used

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  • Synthesis process method and device of 4-acetophenetidine bulk drug
  • Synthesis process method and device of 4-acetophenetidine bulk drug

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Raw material ratio: the molar ratio of p-aminophenethyl ether: acetic anhydride: glacial acetic acid is: 1: 0.5: 0.75;

[0033] Proportion of raw materials: p-aminophenethyl ether (98.0% content) 160kg, acetic anhydride (99.0% content) 73.6L, glacial acetic acid (99.80% content) 120L.

[0034] The synthetic production process of the p-acetamidophenetole of this embodiment concrete procedure is as follows:

[0035] (1) Etification reaction process: First, according to the above-mentioned ratio of ingredients, after measuring and weighing p-aminophenethyl ether, acetic anhydride, and glacial acetic acid, first add 100L of glacial acetic acid to the reaction kettle, heat up to boiling, and add p-aminophenethyl ether to In the reaction kettle, after stirring for 3 minutes, heat up to boiling, reduce the pressure of the reaction kettle to 0.25MPa through the chain pressure of the steam valve, control the temperature in the kettle at 124±3℃, and then increase it by 0.05MPa ev...

Embodiment 2

[0041] Raw material ratio: the molar ratio of p-aminophenethyl ether: acetic anhydride: glacial acetic acid is: 1: 0.46: 0.72;

[0042] Feeding amount: p-aminophenethyl ether (98.0% content) 140kg; acetic anhydride (99.0% content) 64.4L; glacial acetic acid (99.80% content) 101L.

[0043] The preparation of para-acetaminophenethyl ether product process described in the present embodiment is by following operation:

[0044] ⑴. Etching reaction process: First, according to the molar ratio of the above ingredients, after weighing p-aminophenethyl ether, acetic anhydride, and glacial acetic acid, first add 86L glacial acetic acid into the reaction kettle, heat up to 100-108°C and boil, Add 140kg of aminophenethyl ether and stir for 3 minutes, then raise the temperature to boiling, reduce the pressure of the reactor to 0.25MPa through the chain pressure of the steam valve, control the temperature in the kettle at 124±2°C, and then increase it by 0.05MPa every 20 minutes, and rise t...

Embodiment 3

[0050] Raw material ratio: p-aminophenethyl ether: acetic anhydride: the molar ratio of glacial acetic acid is: 1.0: 0.5: 1.16.

[0051]Feeding amount: p-aminophenethyl ether (98.0% content) 100kg; acetic anhydride (99.0% content) 36.1L, glacial acetic acid (99.80% content) 49.7L.

[0052] Present embodiment makes p-acetamidophenetole product technological method by following operation:

[0053] (1) Etification reaction process: First, according to the molar ratio of the above-mentioned ingredients, after weighing p-aminophenethyl ether, acetic anhydride, and glacial acetic acid, add 85% of the total amount of glacial acetic acid to the reaction kettle, heat up to boiling, and add the Add aminophenethyl ether to the reactor, stir for 2-3 minutes, then raise the temperature to boiling, reduce the pressure of the reactor to 0.25MPa through the chain pressure of the steam valve, control the temperature in the reactor at 124±1°C, and then increase it every 20 minutes 0.05MPa, whe...

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Abstract

The invention provides a synthesis process method and device for a 4-acetophenetidine bulk drug, belongs to the technical field of preparation of raw material drugs, and aims to solve the problems that an existing synthesis method for 4-acetophenetidine is complex in process and the used raw material is limited. The 4-acetophenetidine bulk drug is prepared from phenetidine and glacial acetic acidas raw materials under the catalytic action of acetic anhydride, wherein the molar ratio of the p-phenetidine to the acetic anhydride to dilute glacial acetic acid is (0.8-1.1): (0.46-0.55): (0.7-1.18); the synthesis method comprises the following steps: (1) carrying out an acetification reaction; (2) coagulating and dissolving; (3) refining and decolorizing; (4) crystallizing and centrifugally dehydrating; (5) drying, sieving and packaging for preparing the 4-acetophenetidine finished product. The synthesis process method is simple and practical, the raw material is easy to obtain, and the method is suitable for synthesizing and preparing the 4-acetophenetidine.

Description

technical field [0001] The invention belongs to a synthesis process method and device of acetaminophenethyl ether raw material drug in the technical field of raw material drug production. Background technique [0002] With the increasing development and progress of the production technology of raw materials, the technical requirements for the synthesis and production of para-acetaminophenethyl ether raw materials are also getting higher and higher. 10 h 13 NO 2 , the chemical name is p-acetamidophenethyl ether, also known as acetyloxyethylaniline, which belongs to an important raw material drug. In the known technology, the existing p-acetaminophenetole raw material drug is mainly prepared from p-nitrochlorobenzene through etherification, reduction and acetylation reactions. Preparation method 1 is: p-acetamidophenetole can be obtained by diethylketone In the method, paracetamol and ethyl iodide are refluxed in the presence of anhydrous potassium carbonate, and Williamson...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/25
CPCC07C231/02C07C233/25
Inventor 李宾段玉新李浩洋高帅华周国红
Owner 李宾
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