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Process and device for acylation reaction of acetaminophen

A technique for the acylation reaction of acetaminophen and acetaminophen, which is applied in the field of pharmaceutical preparations, can solve the problems of high concentration of acetic acid, high reaction temperature, and long reaction time, and achieve the reduction of waste acid evaporation, lower reaction temperature, The effect of shortening the reaction time

Inactive Publication Date: 2015-12-16
ANQIU LUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The reaction temperature of the conventional acylation process is high, and the waste dilute acid produced is more, and the concentration of acetic acid in the dilute acid is relatively high, resulting in waste of raw materials, long reaction time and low yield

Method used

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  • Process and device for acylation reaction of acetaminophen

Examples

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Comparison scheme
Effect test

Embodiment 1

[0030] Paracetamol acylation process of the present invention is as follows:

[0031] (1) Preparation of materials: Add 1200Kg of para-aminophenol, 2400L of paracetamol mother liquor and 1000Kg of glacial acetic acid into the reactor 1;

[0032] Paracetamol mother liquor comprises the component of following parts by weight:

[0033] 9~11 parts of acetaminophen

[0034] p-Aminophenol≤0.02 parts

[0035] 53~54 parts of acetic acid

[0036] 35~37 parts of water.

[0037] (2) Acylation reaction: raise the temperature of reactor 1 to 108°C to carry out the reaction;

[0038] (3) Distillation of acetic acid: the acid evaporated from the reaction kettle 1 enters the rectification tower 2, the temperature of the bottom of the rectification tower 2 is 108°C, the temperature at the top of the tower is 90°C, and the reflux ratio is 1:9;

[0039] (4) Recovery of dilute acid: dilute acid evaporated from rectification tower 2 enters condenser 3 and condenses to become waste dilute acid...

Embodiment 2

[0047] Paracetamol acylation process of the present invention is as follows:

[0048] (1) Preparation of materials:

[0049] Add 1200Kg of para-aminophenol, 2400L of paracetamol mother liquor and 1000Kg of glacial acetic acid in the reaction kettle 1

[0050] Paracetamol mother liquor comprises the component of following parts by weight:

[0051] 9~11 parts of acetaminophen

[0052] p-Aminophenol≤0.02 parts

[0053] 53~54 parts of acetic acid

[0054] 35~37 parts of water.

[0055] (2) Acylation reaction: raise the temperature of reactor 1 to 132°C to carry out the reaction;

[0056] (3) Distillation of acetic acid: the acid evaporated from the reaction kettle 1 enters the rectification tower 2, the temperature of the bottom of the rectification tower 2 is 108°C, the temperature at the top of the tower is 90°C, and the reflux ratio is 1:9;

[0057] (4) Recovery of dilute acid: dilute acid evaporated from rectification tower 2 enters condenser 3 and condenses to become wa...

Embodiment 3

[0065] A device for realizing the process described in Example 1 and Example 2 consists of a reactor 1, a rectifying column 2 and a condenser 3 connected in sequence.

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Abstract

The invention belongs to field of medicine preparation, and particularly relates to an acylation reaction of acetaminophen. A process for the acylation reaction of acetaminophen comprises the following steps: material preparation, acylation reaction, rectification with acetic acid; recovery of olefine acid, spin-filtering, recovery of a mother solution of acetaminophen, washing and drying. A device for the acylation reaction of acetaminophen is characterized by arranging a rectifying tower between a reaction vessel and a condenser. According to the process, the reaction temperature is reduced, so that the reaction can be carried out below 108 DEG C; the reaction time is shortened to 8.5h; the steam amount of waste acid is reduced by 25%; and the cost of secondary treatment is reduced. The concentration of acetic acid in the waste diluted acid is reduced, and the concentration of waste diluted acid is 50%. The use ratio of raw materials is improved; the cost is saved; and the yield is increased.

Description

technical field [0001] The invention belongs to the field of pharmaceutical preparations, in particular to acetaminophen acylation reaction. Background technique [0002] Acetaminophen (paracetamol or acetaminophen), molecular formula C 8 h 9 NO 2 , usually a white crystalline powder, also known as paracetamol, acetaminophen or paracetamol, is a commonly used antipyretic and analgesic drug, often used for cold fever, joint pain, neuralgia, migraine, cancer pain and Pain relief after surgery, etc. It is the main ingredient in many cold and pain medicines. It is obtained by acylation of p-aminophenol with acetic acid. [0003] The reaction temperature of the conventional acylation process is high, and the waste dilute acid produced is more, and the concentration of acetic acid in the dilute acid is relatively high, resulting in waste of raw materials, long reaction time and low yield. Contents of the invention [0004] The object of the present invention is to provide ...

Claims

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Application Information

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IPC IPC(8): C07C233/25C07C231/02C07C231/24
Inventor 栾汝兴李敏李庆文
Owner ANQIU LUAN PHARMA
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