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Method for synthesizing carbazole compounds

A technology of compound and carbazole, which is applied in the field of synthesizing carbazole compounds, can solve the problem of high cost and achieve the effects of low cost, high reaction yield and product purity, high conversion rate and selectivity

Inactive Publication Date: 2012-08-15
NANTONG HAIDI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The catalytic dehydrogenation efficiency of 1,2,3,4-tetrahydrocarbazole is related to the amount and type of catalyst, the type of solvent, and reaction conditions. After a lot of theoretical and experimental research, it has industrial application prospects, but There is also the problem of high cost

Method used

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  • Method for synthesizing carbazole compounds
  • Method for synthesizing carbazole compounds
  • Method for synthesizing carbazole compounds

Examples

Experimental program
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Embodiment 1

[0049] In a 1000ml three-necked flask equipped with a reflux condenser, add 1,2,3,4-tetrahydrocarbazole 112g (0.66mol), 400g solvent N,N-dimethylformamide successively, add 3.0g activated carbon, Warm to reflux. Heat preservation reaction for 3.0h, filter, wash the catalyst with 50ml hot solvent, combine the filtrate, add 0.5g 10% platinum / mesoporous carbon to it after the filtrate is cooled, raise the temperature to reflux, heat preservation reaction for 5h, filter out the catalyst, distill and concentrate the filtrate, add water , filtered, and dried to obtain 106 g of carbazole with a yield of 97% and a HPLC chromatographic purity of 99%.

Embodiment 2

[0051] In a 1000ml three-necked flask equipped with a reflux condenser, 112g (0.66mol) of 1,2,3,4-tetrahydrocarbazole, 400g of solvent N,N-dimethylacetamide were added successively, and 3.0g of diatomaceous earth was added , warmed to reflux. Heat preservation reaction for 3.0h, filter, 50ml hot solvent washes the catalyst, combine the filtrate, after the filtrate is cooled, add 0.5g 10% ruthenium / activated carbon to it, heat up to reflux, heat preservation reaction for 7h, filter out the catalyst, distill and concentrate the filtrate, add water, After filtering and drying, 105 g of carbazole was obtained with a yield of 96% and a HPLC chromatographic purity of 98.5%.

Embodiment 3

[0053] In a 1000ml three-necked flask equipped with a reflux condenser, 112g (0.66mol) of 1,2,3,4-tetrahydrocarbazole, 400g of solvent polychlorobenzene, and 3.0g of Raney nickel were added in sequence, and the temperature was raised to reflux. Heat preservation reaction for 3.0 hours, filter, wash the catalyst with 50ml of hot solvent, combine the filtrate, add 0.5g 10% ruthenium / alumina to it after the filtrate is cooled, heat up to reflux, heat preservation reaction for 8 hours, distill and concentrate the filtrate, add water, filter and dry , to obtain 103g carbazole, yield 94%, HPLC chromatographic purity 98.1%.

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Abstract

The invention relates to the technical field of preparation of carbazole compounds, in particular to a method for synthesizing carbazole compounds, which includes: obtaining a product by using 1, 2, 3, 4-tetrahydrocarbazole compound as raw materials by means of catalytic dehydrogenation, and leading cheap catalyst and high-activity catalyst to undergo combinatorial catalysis in the catalytic dehydrogenation process: the cheap and low-activity catalyst is used for catalysis at the first step, and then the high-activity catalyst is used for catalysis at the second step; or the high-activity catalyst is used for catalysis at the first step, and then the cheap and low-activity catalyst is used for catalysis at the second step. The method for synthesizing the carbazole compounds is small in catalyst use amount, low in cost and high in reacting conversion rate and selectivity, the content of carbazole is higher than 99%, solvent and the catalyst can be recovered and used indiscriminately, and the method is suitable for industrial production and has the advantages of simple process, high reacting yield, high product purity and environmental friendliness.

Description

technical field [0001] The invention relates to the technical field of preparation of carbazole compounds, in particular to a method for synthesizing carbazole compounds. It belongs to the field of fine chemicals. Background technique [0002] Carbazole compounds are an important class of fine chemical intermediates, widely used in the fields of dyes, pigments, medicines and pesticides, especially for the preparation of high-grade organic pigments. In recent years, the research and application of carbazole and its derivatives are being further deepened, and the demand for carbazole is also increasing. [0003] Carbazole is mainly derived from coal tar, but its separation and refining process is complex, energy consumption is high, product purity is low, and the output is limited, which cannot meet market demand. There are a lot of literature methods about synthesizing carbazole, and Fisher method synthesizing carbazole is one of the most industrialized prospect methods, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/86
CPCY02P20/584
Inventor 倪海平侯启军顾耀张耀叔钱岳
Owner NANTONG HAIDI CHEM
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