A kind of preparation method of electroluminescent organic material O-MeO-DMBI-I

文档序号:1750661 发布日期:2019-11-29 浏览:39次 中文

阅读说明:本技术 一种有机电致发光材料O-MeO-DMBI-I的制备方法 (A kind of preparation method of electroluminescent organic material O-MeO-DMBI-I ) 是由 陆林林 于 2019-09-19 设计创作,主要内容包括:本发明属于有机光电材料技术领域,涉及一种有机电致发光材料O-MeO-DMBI-I的制备方法,步骤在于:①将2-(2-羟苯基)苯并咪唑、氢氧化钾溶液和甲醇充分混合,在惰性气体的保护下滴加碘甲烷,室温反应12小时,得到反应液;②将反应液过滤得到滤饼,真空干燥,得干燥粉末;③将粉末过层析柱,用石油醚/乙酸乙酯混合液淋洗,得到白色晶体。本发明的原料成本较低,反应条件温和,产品收率高,适合放大生产。(The invention belongs to organic photoelectrical material technical fields; it is related to the preparation method of electroluminescent organic material O-MeO-DMBI-I a kind of; step is: being 1. sufficiently mixed 2- (2- hydroxyphenyl) benzimidazole, potassium hydroxide solution and methanol; iodomethane is added dropwise under the protection of inert gas; room temperature reaction 12 hours, obtains reaction solution;2. filter cake is obtained by filtration in reaction solution, it is dried in vacuo, obtains dried powder;3. powder is crossed chromatographic column, is eluted with petrol ether/ethyl acetate mixed liquor, obtain white crystal.Cost of material of the invention is lower, and reaction condition is mild, and product yield is high, is suitble to amplification production.)

1. a kind of preparation method of electroluminescent organic material O-MeO-DMBI-I, it is characterised in that include the following steps:

1. 2- (2- hydroxyphenyl) benzimidazole, potassium hydroxide solution and methanol is sufficiently mixed, dripped under the protection of inert gas Add iodomethane, reacts at room temperature 12 hours, obtain reaction solution;

2. filter cake is obtained by filtration in reaction solution, it is dried in vacuo, obtains dried powder;

3. powder is crossed chromatographic column, is eluted with petrol ether/ethyl acetate mixed liquor, obtain white crystal.

2. synthetic method according to claim 1, it is characterised in that: the step 1. every gram of 2- (2- hydroxyphenyl) benzo miaow Azoles and 1mol potassium hydroxide and 2ml methanol dissolve.

3. synthetic method according to claim 1, it is characterised in that: the step is 1. with thin layer chromatography judgement reaction Terminal, solvent used compare mixture for the 5:1 mass of ethyl acetate and petroleum ether.

4. synthetic method according to claim 1, it is characterised in that: 3. the step elutes chromatographic column in five times, leaching The volume ratio of petroleum ether and ethyl acetate is respectively 50:1,40:1,30:1,20:1,10:1 in dilution.

Technical field

The present invention relates to organic photoelectrical material technical field, in particular to a kind of electroluminescent organic material O-MeO- The preparation method of DMBI-I.

Background technique

Organic electroluminescence device (Organic Light-Emitting Devices, OLEDs) have it is ultra-thin, light, The advantages that luminous efficiency is high, driving voltage is low, fast response time, rich in color, visual angular width, has in display and lighting area Very wide application prospect has started huge research boom in the world in recent years.

Organic electroluminescent phenomenon, which refers to, to be stimulated under electric field action in organic semiconductor luminescent material and gives off light The phenomenon that in research of the illumination with white light OLED s, from the angle of OLED material, there are three types of key techniques, respectively It is luminous (Multi-Photon Emission, the MPE) technology of low-work voltage technology, Phosphorescent OLED technology and multi-photon.And its In low-work voltage technology refer to since the operating voltage and energy consumption of OLEDs are directly directly proportional, it is therefore necessary to pass through reduction The operating voltage of OLED is " economical " luminous to realize.Therefore the reduction of OLEDs power consumption has important practical significance.

O-MeO-DMBI-I English name is 2- (2-methoxyphenyl) -1,3-dimethyl-1H- Benzoimidazol-3-ium iodide, structural formula are as follows:

Therefore, it is necessary to develop the new synthetic method of one kind to improve yield.

Summary of the invention

The main purpose of the present invention is to provide the few a kind of electroluminescent organic material O- of a kind of product yield height, impurity The preparation method of MeO-DMBI-I.

The present invention is achieved through the following technical solutions above-mentioned purpose: a kind of electroluminescent organic material O-MeO-DMBI-I's Preparation method includes the following steps:

1. 2- (2- hydroxyphenyl) benzimidazole, potassium hydroxide solution and methanol is sufficiently mixed, in the protection of inert gas Lower dropwise addition iodomethane reacts at room temperature 12 hours, obtains reaction solution;

2. filter cake is obtained by filtration in reaction solution, it is dried in vacuo, obtains dried powder;

3. powder is crossed chromatographic column, is eluted with petrol ether/ethyl acetate mixed liquor, obtain white crystal.

Specifically, 1. every gram of 2- (2- hydroxyphenyl) benzimidazole and 1mol potassium hydroxide and 2ml methanol dissolve the step.

Specifically, the step is 1. with the terminal of thin layer chromatography judgement reaction, solvent used is ethyl acetate and stone The 5:1 mass of oily ether compares mixture.

Specifically, 3. the step elutes chromatographic column in five times, the volume of petroleum ether and ethyl acetate in eluent solution Than being respectively 50:1,40:1,30:1,20:1,10:1.

Compared with prior art, the preparation method of electroluminescent organic material O-MeO-DMBI-I of the invention a kind of has Beneficial effect is:

Cost of material of the invention is lower, and reaction condition is mild, and product yield is high, is suitble to amplification production.

Detailed description of the invention

Fig. 1 is the nuclear magnetic spectrogram of O-MeO-DMBI-I.

Specific embodiment

A kind of preparation method of electroluminescent organic material O-MeO-DMBI-I, includes the following steps:

1. 2- (2- hydroxyphenyl) benzimidazole, potassium hydroxide solution and methanol is sufficiently mixed, in the protection of inert gas Lower dropwise addition iodomethane reacts at room temperature 12 hours, obtains reaction solution.

The chemical equation of step 1. indicates are as follows:

2. filter cake is obtained by filtration in reaction solution, it is dried in vacuo, obtains dried powder.

3. powder is crossed chromatographic column, is eluted with petrol ether/ethyl acetate mixed liquor, obtain white crystal.

Invention is further described in detail combined with specific embodiments below.

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