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Preparation method and application of metal organic cage compound

A cage compound and metal-organic technology, which is applied in the field of preparation of metal-organic cage compounds, can solve problems such as poor product quality, environmental hazards, and complicated processes, and achieve the effects of high yield, low price, and stable chemical properties

Active Publication Date: 2020-07-28
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chlorosulfonic acid method often produces many toxic and harmful gases, and the pollution problem is serious
In addition, the poor quality of the actual products and low economic benefits lead to the gradual elimination of this method
At present, the process route of the carbon disulfide method is relatively common. Carbon disulfide itself is volatile and difficult to store. It is irritating and flammable at high temperature, which is harmful to human health. It is a poison that damages human nerves and blood vessels. In addition, this production process is complex and harmful to the environment. and many other deficiencies

Method used

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  • Preparation method and application of metal organic cage compound
  • Preparation method and application of metal organic cage compound
  • Preparation method and application of metal organic cage compound

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 4-amino-N-methylbenzamide (15.0g, 100mmol), methyl propiolate (16.8g, 200mmol) and benzaldehyde (10.6g, 100mmol) were added to 20mL of acetic acid, at 80°C Stir under the conditions for 1h, then cool the reaction solution and add it to 200mL of ice water, continue to stir for 1h, filter with suction, wash the filter cake with 300mL of ether, then recrystallize the filter cake with 100mL of ethanol to obtain a yellow powder (24.1g, yield 60%). 1 H-NMR (400MHz, CDCl 3 ):δ7.89(d,2H),7.74(s,2H),7.37(d,4H),7.31-7.27(m,1H),7.20(t,1H),6.21(d,1H),4.99( s,1H), 3.69(s,6H), 3.07(d,3H).

[0024] Weigh the yellow powder (12.18g, 30mmol) and mix with 150mL hydrazine hydrate, reflux and stir for 12h at 85°C, after the reaction, the product is suction filtered, and the filter cake obtained by suction filtration is washed with ethanol, and the filter cake after vacuum drying is dried. A white powder (5.79 g, 48% yield) was obtained. 1 H-NMR (400MHz, DMSO-d 6 ,ppm):δ9.17(s,2H),8.35(...

Embodiment 2

[0028] Weigh ligand H 2 ZPA (58.4mg, 0.1mmol) and Zn(NO 3 ) 2 ·6H 2 O (29.7mg, 0.1mmol) was added to 10mL of a mixed solvent of methanol and dichloromethane with a volume ratio of 1:1, stirred at room temperature for 4h, stirred and filtered, and the filtrate was left standing at room temperature for 2 weeks, and then the solution precipitated Yellow solid, the target compound Zn-ZPA (30.0 mg, yield 40%) can be obtained. Zn 4 C 132 h 112 N 32 o 12 ESI-MS:m / z:864.53[H 3 Zn 4 (ZPA) 4 ] 3+ ,1296.29[H 2 Zn 4 (ZPA) 4 ] 2+ .

Embodiment 3

[0030] Weigh ligand H 2 ZPA (58.4mg, 0.1mmol) and Zn(ClO 4 ) 2 ·6H 2 O (37.2mg, 0.1mmol) was added to 10mL of a mixed solvent of methanol and dichloromethane with a volume ratio of 1:1, stirred at room temperature for 4h, after stirring and filtering, the filtrate was left at room temperature for 2 weeks, and then precipitated out of the solution Yellow solid, the target compound Zn-ZPA (32.4 mg, yield 43.2%) can be obtained. Zn 4 C 132 h 112 N 32 o 12 ESI-MS:m / z:864.53[H 3 Zn 4 (ZPA) 4 ] 3+ ,1296.29[H 2 Zn 4 (ZPA) 4 ] 2+ .

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Abstract

The invention belongs to the technical field of fine chemical engineering, and relates to a preparation method and application of a metal organic cage compound. According to the preparation method, Zn<2+> in transition metal salt is used as a node, L is used as a ligand, and a reaction is conducted to prepare the metal organic cage compound; a synthetic route is that Zn<2+> and L produce Zn-L; theligand L is H<2>ZPA; and the transition metal salt is one selected from a group consisting of zinc perchlorate, zinc nitrate, zinc tetrafluoroborate and zinc trifluoromethanesulfonate. The metal organic cage compound prepared by using the method is low in raw material price, high in yield, stable in chemical property, easy to put into practical application, and capable of efficiently catalyzing cyclobutanone to prepare butyrolactone and catalyzing selective oxidation of thioether to prepare sulfoxide under the condition of mild illumination.

Description

technical field [0001] The invention relates to a preparation method and application of a metal-organic cage compound, which belongs to the technical field of fine chemicals. Background technique [0002] The butyrolactone compounds produced by the oxidation of cyclobutanone are one of the most important intermediates in the chemical industry. Butyrolactone compounds are important raw materials in the pharmaceutical industry, which can be used to manufacture erythromycin derivatives, acetylspiramycin and other antibiotics, and can also synthesize ciprofloxacin, naofukang, vitamins and other medicines; in pesticides In the industry, it is used to produce agricultural chemicals such as chlorophenoxybutyric acid herbicides, indole butyric acid and other insecticides and fungicides; in the chemical fiber industry, lactone compounds can be used as a spinning agent for acrylonitrile fibers Silk solvent, it can also be used as dyeing aid for acrylonitrile, nylon, wool and other fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14B01J31/22C07D307/33C07C315/02C07C317/14
CPCC07D401/14B01J31/2217C07D307/33C07C315/02B01J35/39C07C317/14
Inventor 段春迎赵亮蔡俊凯李亚楠魏建伟
Owner DALIAN UNIV OF TECH
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