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
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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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