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A kind of preparation method and application of PD catalyst with nanoporous structure

A nanoporous, catalyst technology, applied in the field of medicine, can solve the problems of easy desorption, reduced catalytic activity, poor effect, etc., and achieve the effect of easy recovery and improved catalytic performance.

Inactive Publication Date: 2016-02-17
SHAOXING UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Our experimental results show that: with Pd-C and Ru-C as catalysts, although the catalytic hydrogenation reaction can obtain products in good yields, the effect of repeated use of Pd-C and Ru-C catalysts is poor
The reason for the poor reuse effect may be that the catalytic active materials Pd and Ru are only loaded on the carbon material through adsorption, and Pd and Ru are easily desorbed during the high-temperature and high-pressure reaction process, so that the Pd-C and Ru-C catalysts Reduced catalytic activity during recycling
Another disadvantage of the catalytic hydrogenation of 6-benzyl-5,7-dioxo-pyrrolo[3,4,b]pyridine using Pd-C and Ru-C as catalysts is that the desorbed Pd and Ru are easy to the product create pollution

Method used

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  • A kind of preparation method and application of PD catalyst with nanoporous structure
  • A kind of preparation method and application of PD catalyst with nanoporous structure
  • A kind of preparation method and application of PD catalyst with nanoporous structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 0.5 g azobisisobutyronitrile, 2.5 ml divinylbenzene, 1.5 g 1,3,5-triacryloylhexahydro-1,3,5-triazine, 0.01 g ferric chloride, 0.025 g persulfate Add ammonium co-initiator to 80 ml tetrahydrofuran in turn, add 3 ml water as a co-solvent, stir at room temperature for 3 hours (stirring rate is about 800rpm), reflux at 100°C for 12 hours, further solvent thermal crystallization, 120°C reactor treatment After 24 hours, take out the reaction kettle, open the cover to evaporate the solvent (humidity is about 60%, evaporate for 24 hours) to obtain the crude product. The residual salt in the sample was removed by washing with water, and vacuum-dried at 80° C. to obtain a nanoporous material with open pores.

[0035] Weigh 2g nanoporous material PDVB-THAT and 0.224gPd(OAc) 2 In 30mL tetrahydrofuran and 10mL water, after stirring at room temperature for 3 hours, add 68mgNaBH 4 to Pd(OAc) 2 to restore. After the reactant was stirred at room temperature for 10 hours, the catalys...

Embodiment 2

[0037] Catalytic hydrogenation of 6-benzyl-5,7-dioxo-pyrrolo[3,4,b]pyridine: add 10g of 6-benzyl-5,7-dioxo-pyrrolo[3, 4,b] pyridine and 100 mL n-butyl acetate, add 1 g PDVB-THATPd 0 (the content of Pd is 5%), the pressure of flushing into hydrogen is 5bar, heating at 50g for 7 hours, filtering, and recovering PDVB-THATPd 0 Catalyst, the filtrate obtains 9.8g light yellow solid after removing the solvent, it is determined as racemic cis-8-benzyl-7,9-dioxo-2,8-diazabicyclo[4 ,3,0] nonane. The yield was 97%.

[0038]

[0039] 1H-NMR (CDCl 3 ,400MHz)δppm7.32–7.24(m,5H),4.64(s,2H),3.84(d,1H,J=6.8Hz),2.89-2.2.83(m,1H),2.82-2.76(m, 1H),2.70-2.64(m,1H),2.08(brs,1H),2.03-1.93(m,1H),1.68–1.61(m,1H),1.54-1.50(m,1H).

Embodiment 3

[0041] The catalyst is reused for the second time: add 10g of 6-benzyl-5,7-dioxo-pyrrolo[3,4,b]pyridine and 100mL of n-butyl acetate in the autoclave, add the catalyst recovered in Example 2 PDVB-THATPd 0 Afterwards, the pressure of flushing hydrogen is 5bar, heated at 50°C for 7 hours, filtered, and recovered PDVB-THATPd 0 Catalyst, the filtrate obtained 9.7g light yellow solid after removing the solvent, and was determined to be racemic cis-8-benzyl-7,9-dioxo-2,8-diazabicyclo[4 ,3,0] nonane. The yield is 95%.

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Abstract

The invention belongs to the technical field of medicine and discloses a preparation method of a Pd catalyst with a nano-porous structure, wherein 8-benzyl-7,9-dioxo-2,8-diazabicyclo[4,3,0]-1-alkenylnonane is prepared by catalytically hydrogenating 6-benzyl-5,7-dioxo-pyrrolo[3,4,b]pyridine with the catalyst. The method comprises the steps of (1) preparing a novel Pd catalyst with nano-porous structural characters, and (2) catalytically hydrogenating 6-benzyl-5,7-dioxo-pyrrolo[3,4,b]pyridine under the condition of a temperature ranging from 50 to 80 DEG C in the presence of the catalyst in an ester solvent or a polar protonic solvent to obtain 8-benzyl-7,9-dioxo-2,8-diazabicyclo[4,3,0]-1-alkenylnonane. The catalyst can be recycled; even after the catalyst is reused for a plurality of times, the catalytic activity of the catalyst cannot be reduced.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of a Pd catalyst with a nanoporous structure, and the catalytic hydrogenation of 6-benzyl-5,7-dioxo-pyrrolo[3,4,b ]pyridine to prepare 8-benzyl-7,9-dioxo-2,8-diazabicyclo[4,3,0]-1-enenonane. Background technique [0002] Moxifloxacin (1, Moxifloxacin) is the fourth-generation quinolone antibacterial drug developed by Bayer Company in Germany. Its trade name is "Baifule", and it is a chiral drug. The drug has an ultra-broad antibacterial spectrum. It not only retains the high activity against Gram aerobic bacteria, but also has very strong antibacterial activity against anaerobic bacteria, mycoplasma, chlamydia, etc., especially against Escherichia coli and Streptomyces aureus Antibiotic-resistant strains showed strong activity. [0003] [0004] The industrial synthesis of the moxifloxacin side chain (2) uses 2,3-dicarboxypyridine (3) as the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06B01J35/10B82Y30/00C07D471/04
CPCY02P20/584
Inventor 齐陈泽冯高峰陈风江何程飞
Owner SHAOXING UNIVERSITY
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