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Catalyzed method for synthesizing 9-ethyl octahydrocarbazole with rufe/n-cnts catalyst

A technology of ethyl octahydrocarbazole and ethyl carbazole, which is applied in the direction of physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, and can solve the problem of 9-ethyl octahydrocarbazole There are few reports on the synthesis method of hydrocarbazole, and the effect of high activity and selectivity is achieved

Active Publication Date: 2020-07-31
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports on the synthetic method of 9-ethyl octahydrocarbazole

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Catalyst preparation process

[0022] 0.02mmol RuCl 3 and 0.024mmol FeCl 3 Dissolve in 10mL distilled water, stir in an ice bath at 0°C for a period of time, then add 4mmol N-CNTs to the above solution, after stirring well, add dropwise 0.1mol / L sodium borohydride solution for reduction for 2h, filter and store at 130°C Dry in a drying oven for 16h, and the catalyst is recorded as RuFe 1.2 / 200N-CNTs, airtight storage.

[0023] Hydrogenation process

[0024] Put 100mg of the above-mentioned catalyst and 10g of 9-ethylcarbazole in a high-pressure reactor, raise the reactor to 160°C, feed hydrogen into the reactor to make the pressure 4.5Mpa, stir and react at a speed of 700rpm for 5h, and react After the analysis, the selectivity of 9-ethyl octahydrocarbazole was 94.4%, and the yield of 9-ethyl octahydrocarbazole was 92.3%.

Embodiment 2

[0026] 0.02mmol RuCl 3 and 0.08mmol FeCl 3 Dissolve in 10mL distilled water, stir in an ice bath at 0°C for a period of time, then add 12mmol N-CNTs to the above solution, after stirring well, add dropwise 0.4mol / L sodium borohydride solution for reduction for 2h, filter and store at 80°C Dry in a drying oven for 9h, the catalyst is recorded as RuFe 4 / 600N-CNTs, airtight storage.

[0027] Hydrogenation process

[0028] Put 100mg of the above catalyst and 10g of 9-ethylcarbazole in a high-pressure reactor, raise the reactor to 120°C, feed hydrogen into the reactor to make the pressure 2.5Mpa, stir and react at 450rpm for 3h, and react After the analysis, the selectivity of 9-ethyl octahydrocarbazole was 89.8%, and the yield of 9-ethyl octahydrocarbazole was 87.2%.

Embodiment 3

[0030] 0.02mmol RuCl 3 and 0.04mmol FeCl 3 Dissolve in 10mL distilled water, stir in an ice bath at 0°C for a period of time, then add 10mmol N-CNTs to the above solution, after stirring thoroughly, add dropwise 0.3mol / L sodium borohydride solution for reduction for 2h, filter and store at 120°C Dry in a drying oven for 14h, and the catalyst is recorded as RuFe 2 / 500N-CNTs, airtight storage.

[0031] Hydrogenation process

[0032] Put 100mg of the above catalyst and 10g of 9-ethylcarbazole in a high-pressure reactor, raise the reactor to 150°C, feed hydrogen into the reactor to make the pressure 4.0Mpa, stir and react at a speed of 600rpm for 4h, and react After the analysis, the selectivity of 9-ethyl octahydrocarbazole was 88.3%, and the yield of 9-ethyl octahydrocarbazole was 85.1%.

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Abstract

The invention discloses a method for catalytic synthesis of 9-ethyloctahydrocarbazole by using a RuFe / N-CNTs catalyst, and belongs to the technical field of chemistry and chemical engineering. The method includes the steps that the prepared RuFe / N-CNTs catalyst and 9-ethylcarbazole are placed in a high pressure reaction still, the reaction still is heated to a certain temperature, and hydrogen isintroduced into the reaction still for carrying out a reaction under stirring for a certain time to obtain 9-ethyloctahydrocarbazole. The RuFe / N-CNTs catalyst is prepared by preparing Ru, Fe and deionized water at a certain molar ratio, adding a carrier N-CNTs to the solution above, and adding a reducing agent to the mixed solution for filtering and drying. The RuFe / N-CNTs catalyst prepared by themethod has higher activity and selectivity. The catalyst is used for hydrogenation of 9-ethylcarbazole to synthesize 9-ethyloctahydrocarbazole, the selectivity is higher than 85.6%, and the yield ismore than 83.7%.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a method for synthesizing 9-ethyloctahydrocarbazole by catalyzing 9-ethylcarbazole with a RuFe / N-CNTs catalyst. Background technique [0002] 9-Ethyl octahydrocarbazole is an important intermediate for the synthesis of anthraquinone organic pigments. It has broad application prospects in the fields of photoelectrochemistry, medicine, dyes, coatings, etc. It has anti-cancer, bactericidal, anti-fungal and mosquito-inhibiting properties and other effects. At present, the synthetic method of 9-ethyl octahydrocarbazole is seldom reported. [0003] 9-Ethylcarbazole is an important hydrogen storage material in Ru / Al 2 o 3 Under the catalyst, hydrogenation can be achieved very well. The hydrogenation product is mainly 9-ethyldodecahydrocarbazole, and the selectivity of the reaction to 9-ethyldodecahydrocarbazole is as high as 98%. During the reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J27/24C07D209/86
CPCB01J23/8906B01J27/24C07D209/86
Inventor 万超王嘉佩姚芳许立信吴胜华雷昭
Owner ANHUI UNIVERSITY OF TECHNOLOGY