A kind of synthesis and purification method of 4-bromo-9-ethylcarbazole

A technology of ethylcarbazole and synthesis method, which is applied in the field of one-step synthesis of carbazole derivatives 4-bromo-9-ethylcarbazole and its purification, and achieves the effect of high-purity preparation

Active Publication Date: 2016-07-06
SHAANXI LIGHTE OPTOELECTRONICS MATERIAL CO LTD
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Problems solved by technology

The preparation method of 4-bromo-9-ethylcarbazole has not been reported in the relevant literature at present. The patent of the present invention realizes the preparation of 4-bromo-9-ethylcarbazole through a one-step method, and obtains the high quality product

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  • A kind of synthesis and purification method of 4-bromo-9-ethylcarbazole
  • A kind of synthesis and purification method of 4-bromo-9-ethylcarbazole

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Embodiment Construction

[0010] The preparation method of 4-bromo-9-ethylcarbazole provided by the present invention in the specific examples will be described below in conjunction with the accompanying drawings.

[0011] Example of a synthetic route for the synthesis of 4-bromo-9-ethylcarbazole:

[0012] Synthesis of 4-bromo-9-ethylcarbazole according to the following reaction formula

[0013] Reaction formula:

[0014]

[0015] Specific synthesis operation method: Weigh 50.0g of 2-bromo-2'-nitro-1,1'-biphenyl, then measure 300ml of triethylphosphite into a 1L three-necked reaction flask, and slowly heat up to 2 -Bromo-2'-nitro-1,1'-biphenyl is completely dissolved, continue to heat up to 80°C~145°C, and the reaction time is 4~24 hours to terminate the reaction.

[0016] After the reaction, distill the reaction solution under reduced pressure at 120°C~145°C (pressure -0.06~-0.08MPa) until no solvent slips out, stop heating, and use the crude product of 4-bromo-9-ethylcarbazole 3 times of silica...

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Abstract

The invention relates to a 4-bromine-9-ethyl carbazole synthesis method through synthesis by a simple one step method and a purifying method thereof, and realizes accurate structural characterization to the prepared product. The 4-bromine-9-ethyl carbazole synthesis method comprises the following steps: dissolving 2-bromine-2'-nitro-1,1'-biphenyl in 5-8 times of triethyl phosphate, reacting at 80-145 DEG C, wherein reaction time is less than 24 hours; performing underpressure distillation on a reaction solution under 120-145 DEG C until no solvent is distilled, and stopping heating to obtain the 4-bromine-9-ethyl carbazole crude product. The 4-bromine-9-ethyl carbazole purifying method comprises the following steps: using 2-3 times of silica gel with 80-120 meshes and 10 times of n-heptane on 4-bromine-9-ethyl carbazole crude product for passing column, and using 3-8 times n-heptane for recrystallization to obtain the 4-bromine-9-ethyl carbazole pure product. The prepared 4-bromine-9-ethyl carbazole is an important intermediate of an organic electroluminescence (EL) device functional material.

Description

technical field [0001] The invention relates to a method for synthesizing carbazole derivative 4-bromo-9-ethylcarbazole in one step and its purification method. Background technique [0002] Organic electroluminescence (EL) is a phenomenon in which organic materials are excited by electrical energy to emit light. In 1987, Dr. Deng Qingyun of Kodak first used the principle of organic electroluminescence to manufacture organic light-emitting diodes (OLEDs). Compared with traditional displays, organic electroluminescent EL displays have attracted much attention because of their advantages such as low driving voltage, strong luminous brightness, high efficiency, fast response, wide viewing angle, and flexible display panels. It is the next generation display after LCD and plasma display. At present, the main problem restricting the development of organic electroluminescence EL is that the lifetime and efficiency of organic light-emitting materials cannot meet the practical req...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/88C07D209/84
CPCC07D209/88
Inventor 王亚龙
Owner SHAANXI LIGHTE OPTOELECTRONICS MATERIAL CO LTD
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