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Synthesis method of azo small molecules for zinc oxide nanoparticle stable ligands

A technology of zinc oxide nanoparticles and nanoparticles, which is applied in the field of material chemistry, can solve problems such as potential safety hazards, and achieve the effects of preventing tailing, good separation effect, and enhanced absorption spectrum

Pending Publication Date: 2022-07-22
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few reports on the synthesis of aminoalcohols substituted azobenzene. The following are the synthesis steps. In this synthesis method, toxic or explosive compounds (such as ammonia, sodium azide, etc.) or strong reduction are commonly used. Agents (lithium aluminum hydride, etc.), there is a great potential safety hazard

Method used

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  • Synthesis method of azo small molecules for zinc oxide nanoparticle stable ligands
  • Synthesis method of azo small molecules for zinc oxide nanoparticle stable ligands
  • Synthesis method of azo small molecules for zinc oxide nanoparticle stable ligands

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[0036] The invention discloses a method for synthesizing an azo-based small molecule used for a nanoparticle stabilizing ligand, comprising the following steps:

[0037] (1) 4-N-phenylbenzamide, potassium carbonate and N,N-dimethylformamide were added to a pre-dried round bottom flask under argon atmosphere, and then N-(6-bromo hexyl)phthalimide and the mixture was stirred at 120°C until the reaction was complete. The resulting suspension was placed in a separatory funnel and some ethyl acetate, chloroform and water were added. Using the organic phase as the raw material and ethyl acetate as the extractant, extract the residue in the aqueous solution. The organic phase was collected and washed with saturated sodium hydroxide solution. The obtained solution was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to obtain an intermediate white solid, as shown in the following formula 1

[0038]

[0039] (2) The ethanol suspension of th...

Embodiment 1

[0044](1) 4-N-Phenylbenzamide (1.88g, 9.47mmol), potassium carbonate (2.35g, 17.0mmol) and N,N-dimethylformamide (50ml) were added to a preliminarily In a dry round bottom flask, N-(6-bromohexyl)phthalimide (2.63 g, 8.5 mmol) was then added and the mixture was stirred at 120°C until the reaction was complete. The resulting suspension was placed in a separatory funnel and 100 mL of ethyl acetate, chloroform and water were added (3:2:5 by volume). Using the organic phase as the raw material and ethyl acetate as the extractant, extract the residue in the aqueous solution. The organic phase was collected and washed with saturated sodium hydroxide solution. The obtained solution was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to obtain a white solid (3.25 g, yield 90%), which was characterized by hydrogen NMR ( figure 1 ), 1 H NMR(500MHz, DMSO-d6)δ7.91-7.84(m,6H),7.71-7.62(m,2H),7.58-7.37(m,2H),6.88-7.05(m,2H),4.03(t , J=6.5Hz, 2H),...

Embodiment 2

[0048] (1) 4-N-Phenylbenzamide (2.15g, 10.85mmol), potassium carbonate (2.70g, 19.5mmol) and N,N-dimethylformamide (50ml) were added to a preliminarily In a dry round bottom flask, N-(6-bromohexyl)phthalimide (2.70 g, 9.8 mmol) was then added and the mixture was stirred at 120°C until the reaction was complete. The resulting suspension was placed in a separatory funnel and 100 mL of ethyl acetate, chloroform and water were added. Using the organic phase as the raw material and ethyl acetate as the extractant, extract the residue in the aqueous solution. The organic phase was collected and washed with saturated sodium hydroxide solution. The resulting solution was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to obtain a white solid (3.45 g, yield 83%).

[0049] (2) The ethanol suspension of the product obtained in step (1) was placed in a pre-dried two-neck round bottom flask. The mixture was heated to 90°C and hydrazine hydrate (...

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Abstract

The invention discloses a synthesis method of azo small molecules for zinc oxide nanoparticle stable ligands. A target molecule AZO-NH2 is synthesized by adopting a two-step method, in the first step, reagents such as 4-phenylazo phenol and N-(6-bromohexyl) phthalimide are used as raw materials to synthesize a white intermediate, in the second step, reagents such as hydrazine hydrate are added into the intermediate obtained in the first step, and the AZO-NH2 is finally obtained through a series of steps such as extraction, drying and column chromatography. Reagents used in the experiment process are all non-toxic reagents, so that the safety of the experiment process can be ensured.

Description

technical field [0001] The invention relates to the field of material chemistry, in particular to a method for synthesizing azo-based small molecules used for stabilizing ligands of zinc oxide nanoparticles. Background technique [0002] Azobenzene molecule is a typical photoisomeric molecule, and its structure will change when irradiated with different wavelengths of light. Azobenzene has been used in many fields such as dyes, drugs, liquid crystal materials, and smart packaging. There are many synthetic methods for azobenzene and its derivatives, including diazo coupling method, nitro reduction method, arylhydrazine oxidation method and arylamine oxidation method. But the synthesis of p-amino alcohols substituted azobenzene is rarely reported. The following is its synthesis step. In this synthesis method, toxic or explosive compounds (such as ammonia, sodium azide, etc.) or strong reduction are commonly used. Agents (lithium aluminum hydride, etc.), there is a great safet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C245/08C01G9/02B82Y40/00B82Y30/00C09K11/02C09K11/54
CPCC07C245/08C07D209/48C01G9/02B82Y40/00B82Y30/00C09K11/025C09K11/54
Inventor 耿家厚王金辉
Owner NINGBO UNIV
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