Preparation method of adamantanol compound

A technology of adamantanol and adamantane methanol, which is applied in the field of preparation of adamantanol compounds, can solve problems such as inability to use sulfuric acid solution, difficult treatment, and excessive waste water, and achieve the effects of environmental friendliness, low cost, and good economic benefits

Active Publication Date: 2015-06-24
四川众邦新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses expensive carbocation products (tert-butanol, tert-butyl chloride, tert-butyl bromide, etc.) many and difficult to handle

Method used

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  • Preparation method of adamantanol compound

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Experimental program
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Effect test

Embodiment 1

[0027] Add 600ml of 20% sodium perchlorate solution in a 1000ml four-necked flask, add 60g of adamantane under stirring, and react at 40°C for 6 hours after adding; Qualitative confirmation was carried out against standard data, and quantitative analysis was carried out with standard products by gas chromatography (GC). At this time, the content of adamantane in the reaction solution was 0.6%, and the content of 1-adamantanol was 98.7%.

[0028] Cool to 5-10°C and stir for 2 hours, filter, wash with 50ml of cold water at 10°C, wash with 30ml of cold ethanol at 10°C, and dry at 90°C to obtain 63.5g of 1-adamantanol with a yield of 94.7%, analyzed by GC The content is 99.8%.

Embodiment 2

[0030] Except that 60g of 1-adamantanol was used instead of adamantane, and the reaction temperature was 70°C, the rest of the operations were the same as in Example 1. As a result, 62.7g of 1,3-adamantanediol was obtained with a yield of 94.5% and a GC analysis content of 99.6%. .

Embodiment 3

[0032] Except that 60 g of 1-methyladamantane was used instead of adamantane, and the reaction temperature was 60° C., the rest of the operations were the same as in Example 1. As a result, 61.8 g of 3-methyl-1-adamantanol was obtained, and the yield was 93.1%. GC analysis The content is 99.7%.

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Abstract

The invention discloses a preparation method of an adamantanol compound. The preparation method is implemented by reacting an adamantane compound with a sodium perchlorate solution at a reaction temperature of 0-100 DEG C so as to obtain the adamantanol compound. The reaction mechanism of the method is as follows: because the +7 valence chlorine of sodium perchlorate has a strong oxidizing property, and can oxidize tertiary carbons on an adamantane ring so as to form hydroxyl, thereby obtaining the adamantanol compound. By using the method, most of the sodium perchlorate solution can be recycled and reused, therefore, the method is extremely low in cost; produced wastewater is greatly reduced, therefore, the method is suitable for industrialized production; a situation that expensive carbocation resultants and organic nitrile compounds are required when other acids such as sulfuric acid are adopted is avoided, and the application of expensive catalysts is also avoided, therefore, the method is low in cost, high in yield and good in economic benefits; and no emission of pollutants such as chromium and the like which seriously pollute the environment is caused, therefore, the method is environment-friendly. The method disclosed by the invention is extremely low in cost; and produced 'three wastes' are greatly reduced, therefore, the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of adamantanol compounds. Background technique [0002] The adamantanol compound obtained by bonding a hydroxyl group on the adamantane skeleton is a very important fine chemical product, which can be used to prepare photoresist monomers, photochromic compounds, pharmaceutical intermediates, etc., and is used in coatings, Adhesives, films, absorbent materials, etc. also have a wide range of uses. [0003] Regarding the preparation method of adamantanol compounds, the known methods mainly include bromination of adamantanes, followed by high-temperature hydrolysis under a certain pressure or using excessive silver sulfate; in the presence of a catalyst, the adamantanes are treated with oxygen ( or air) oxidation; use chromium trioxide in acetic acid to oxidize adamantanes; react adamantanes with sulfuric acid and organic nitrile compounds, and then hydrolyze; react adamantanes with oleum to form adamantane s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/37C07C29/48
CPCC07C29/48C07C2603/74C07C35/37
Inventor 史翔张鸿傅绍莲牟敏
Owner 四川众邦新材料股份有限公司
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