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Preparation and purification method of 6-chloro-5-amino o-cresol

A technology of amino-o-cresol and purification method, which is applied in the field of preparation and purification of 6-chloro-5-amino-o-cresol, can solve the problem that the purification method is not mentioned in public documents, and achieves good quality and high yield Effect

Inactive Publication Date: 2020-05-08
常熟市联创化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the synthesis method of 6-chloro-5-amino-o-cresol, and the purification method of the substance has not been mentioned in the open literature.

Method used

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  • Preparation and purification method of 6-chloro-5-amino o-cresol
  • Preparation and purification method of 6-chloro-5-amino o-cresol
  • Preparation and purification method of 6-chloro-5-amino o-cresol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Put 500 kg of methanol, 100 kg of 6-chloro-5-nitro-o-cresol and 1 kg of 5% palladium carbon into a 1000-liter high-pressure hydrogenation kettle, replace the air in the kettle with nitrogen three times, and then replace the nitrogen with hydrogen. Pass hydrogen to react, control the internal temperature at 60°C, and the pressure in the kettle at 0.2MPa.

[0034] Keep warm for 2.5h to stop the reaction. Filter under nitrogen pressure to remove the catalyst. The resulting filtrate enters the solvent recovery tank. Open the steam and recover the solvent methanol.

[0035] After recovery, about 78.4 kg of crude product of 6-chloro-5-nitro-o-cresol was obtained by drying.

[0036] In a 100-liter sublimation kettle, put 70 kg of the above-mentioned crude product of 6-chloro-5-amino-o-cresol, control the internal temperature at 100°C, and feed nitrogen gas with a nitrogen flow rate of 45 L / min. The sublimation material is smashed, and the sublimation time is about 10 hours...

Embodiment 2

[0039] Put 600 kg of methanol, 100 kg of 6-chloro-5-nitro-o-cresol and 5 kg of 5% palladium carbon into a 1000-liter high-pressure hydrogenation kettle, replace the air in the kettle with nitrogen three times, and then replace the nitrogen with hydrogen. Pass hydrogen to react, control the internal temperature at 80°C, and the pressure in the kettle is 0.4MPa.

[0040] Keep warm for 5h, stop the reaction. Filter under nitrogen pressure to remove the catalyst. The resulting filtrate enters the solvent recovery tank. Open the steam and recover the solvent methanol.

[0041] After recovery, about 75.9 kg of crude product of 6-chloro-5-nitro-o-cresol was obtained by drying.

[0042] In a 100-liter sublimation kettle, put 70 kg of the above-mentioned 6-chloro-5-amino-o-cresol crude product, control the internal temperature at 135°C, feed nitrogen gas, and the nitrogen flow rate is 65L / min. The sublimates are smashed, and the sublimation time is about 2 hours until the product i...

Embodiment 3

[0045] Put 550 kg of ethanol, 100 kg of 6-chloro-5-nitro-o-cresol and 1 kg of 5% palladium carbon into a 1000-liter high-pressure hydrogenation kettle, replace the air in the kettle with nitrogen three times, and then replace the nitrogen with hydrogen. Pass hydrogen to react, control the internal temperature at 70°C, and the pressure in the kettle at 0.2MPa.

[0046] Keep warm for 5h, stop the reaction. Filter under nitrogen pressure to remove the catalyst. The resulting filtrate enters the solvent recovery tank. Open the steam and recover the solvent methanol.

[0047] After recovery, about 77.5 kg of crude product of 6-chloro-5-nitro-o-cresol was obtained by drying.

[0048] In a 100-liter sublimation kettle, put 70 kg of the above-mentioned 6-chloro-5-amino-o-cresol crude product into it, control the internal temperature at 110°C, and feed nitrogen gas with a nitrogen flow rate of 50 L / min. The sublimation is broken, and the sublimation time is about 5.5 hours until th...

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Abstract

The invention discloses a preparation method of 6-chloro-5-amino-o-cresol. The method comprises the following steps: carrying out catalytic hydrogenation on 6-chloro-5-nitro-o-cresol used as an initial raw material to obtain a 6-chloro-5-amino-o-cresol crude product; and carrying out nitrogen-assisted sublimation on the obtained crude product, and crushing to directly obtain a finished product. The method has the advantages that refining and purifying of the crude product with an organic solvent is avoided, and the method is high in yield, good in quality, safe and environment-friendly.

Description

technical field [0001] The invention relates to the field of fine organic synthesis, in particular to a method for preparing and purifying 6-chloro-5-amino-o-cresol. Background technique [0002] 6-Chloro-5-amino-o-cresol can be used as a coupling agent in the components of permanent oxidative hair dyes. It combines with many color-developing bases under the action of oxidants to form the final dye molecule, which is locked inside the hair. [0003] As a hair dye pigment allowed in the 2015 edition of the "Safety and Technical Specifications for Cosmetics", 6-chloro-5-amino-o-cresol is widely used in various oxidative hair dye formulations. [0004] [0005] In some newly developed technical patents, 6-chloro-5-amino-o-cresol is further reacted with other color bases and used as a new type of pigment (such as: WO2009077390 (A2), JP201629178 (A), etc. ). [0006] In addition, there is also a patent disclosing a method for synthesizing anticancer drugs using 6-chloro-5-am...

Claims

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Application Information

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IPC IPC(8): C07C213/02C07C215/76C07C213/10
CPCC07C213/02C07C213/10C07C215/76
Inventor 陈龙
Owner 常熟市联创化学有限公司
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