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Method for preparing 2-amido-4,6-dichlorophenol

A technology of dichlorophenol and nitrophenol, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxyl compounds, etc., can solve the problems that the preparation method has not yet been developed, and achieve easy recovery and application, easy availability of raw materials, The effect of easy operation

Active Publication Date: 2013-08-14
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the preparation method of 2,4-dichloro-6-nitrophenol has not yet been developed

Method used

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  • Method for preparing 2-amido-4,6-dichlorophenol
  • Method for preparing 2-amido-4,6-dichlorophenol
  • Method for preparing 2-amido-4,6-dichlorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 2.0g NiCl 2 Dissolve in 6.5mL distilled water, add 5g SiO to the beaker 2 (BET specific surface area = 198m 2 / g), soaked overnight, stirred in a 343K water bath until dry, baked at 373K for 6 hours, and roasted at 473K for 4 hours for later use. Under a 333K water bath, add 32.5mL of methanol, 5mL of ethanol, 7.5mL of hydrazine hydrate, 1.0g of sodium hydroxide, 1.0mL of distilled water and 1.0g of potassium borohydride into the three-necked flask, stir until dissolved, and weigh a certain amount of catalyst precursor The body was poured into a three-necked flask to obtain Ni-B / SiO 2 The samples were washed repeatedly with distilled water and ethanol in turn, and finally stored in ethanol for future use.

[0026] Add catalyst wet weight 2.35g, 2,4-dichloro-6-nitrophenol 7.5g and 150mL ethanol successively in 500ml autoclave, successively replace with nitrogen, hydrogen respectively 3 times, to remove air, pass into H 2 to 0.5MPa. Start stirring, the stirring...

Embodiment 2

[0028] Catalyst preparation operation process is the same as Example 1. SiO 2 (BET specific surface area = 198m 2 / g) is 5.0g, NiCl 2 2.0g, methanol 32.5mL, ethanol 5mL, hydrazine hydrate 7.5mL, sodium hydroxide 0.17g, distilled water 1.25mL and potassium borohydride 1.25g.

[0029] In a 500mL autoclave, 2.2g of catalyst wet weight, 7.5g of 2,4-dichloro-6-nitrophenol and 150ml of ethanol were successively added, followed by replacement with nitrogen and hydrogen for 3 times respectively to remove the air, and introduce H 2 to 0.6MPa. Start stirring, the stirring speed is 800r / min, and the autoclave is slowly heated to 333K. The reaction process was monitored by observing and recording the change of the pressure in the autoclave with time, and when the pressure no longer changed, the reaction was continued for 10 minutes and then stopped. Extract the solution in the kettle, filter out the catalyst (to be used mechanically next time), evaporate the filtrate to dryness under...

Embodiment 3

[0031] Catalyst preparation operation process is the same as Example 1. SiO 2 (BET specific surface area = 198m 2 / g) is 5.0g, NiCl 2 2.0g, baked at 373K for 6 hours, roasted at 573K for 4 hours, methanol 32.5mL, ethanol 5mL, hydrazine hydrate 7.5mL, sodium hydroxide 0.17g, distilled water 1.25mL and potassium borohydride 1.25g.

[0032]In a 500mL autoclave, 2.35g of catalyst wet weight, 7.5g of 2,4-dichloro-6-nitrophenol and 150mL of propanol were sequentially added, replaced with nitrogen and hydrogen for 3 times in order to remove the air, and introduced H 2 to 0.5MPa. Start stirring, the stirring speed is 800r / min, and the autoclave is slowly heated to 343K. The reaction progress was monitored by observing and recording the change of the pressure in the autoclave with time, and when the pressure no longer changed, the reaction was continued for 10 minutes and then stopped. Extract the solution in the kettle, filter out the catalyst (to be used mechanically next time),...

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Abstract

The invention relates to a method for preparing 2-amido-4,6-dichlorophenol. The method comprises the following steps of: adding a Ni-B / SiO2 amorphous catalyst, 2,4-dichloro-6-nitrophenol and a polar solvent into an autoclave in turn; replacing air by using nitrogen and hydrogen in turn; introducing H2 until the pressure is between 0.5 and 1.0Mpa; heating the autoclave in a water bath to 333-353K;starting stirring, adjusting the stirring rotating speed more than or equal to 500r / min, continuously reacting for 10min when the pressure does not change; and extracting solution in the autoclave, filtering out the catalyst, and drying the product in vacuum after the filtrate is decompressed and distilled. The method for preparing the 2-amido-4,6-dichlorophenol by adopting the Ni-B / SiO2 amorphous catalyst requires small hydrogen pressure and less equipment investment, and the solvent and the catalyst can be recycled, so that the continuously pollution-free production for preparing the 2-amido-4,6-dichlorophenol is realized.

Description

technical field [0001] The invention relates to a preparation method of 2-amino-4,6-dichlorophenol, which belongs to the field of chemical industry and chemical medicine. Background of the invention [0002] 2-amino-4,6-dichlorophenol (2-amino-4,6-dichlorophenol) is also known as "2,4-dichloro-6-aminophenol", and its structural formula is: [0003] [0004] 2-amino-4,6-dichlorophenol is an important fine chemical intermediate, which is widely used in the production of fine chemicals such as dyes and organic synthesis. In 1967, U.S. Patent 3,349,090 reported that it was an essential raw material for the synthesis of the medicine losamide for the treatment of schistosomiasis in swine, cattle and sheep; in 1987, U.S. Patent 244,196 reported that 2-amino-4,6-dichlorophenol was used as a synthetic compound containing cyanoformazan ( Determination of magnesium ions) intermediate; reported in 2005 US Patent 20050124667 as an important intermediate for the synthesis of plasminog...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/76C07C213/02
CPCY02P20/584
Inventor 邱滔毛庆磊吕新宇田华
Owner 溧阳常大技术转移中心有限公司
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