Method for preparing 1-adamantanol

A technology of adamantanol and chloroadamantane, which is applied in the field of preparation of 1-adamantanol, can solve the problems of unfavorable industrial production, long reaction time, complex process, etc., and achieve improved production efficiency, low environmental pollution, and post-processing simple effect

Active Publication Date: 2017-05-31
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Bromine is used as a halogenating agent, and its dosage needs to be 1 to 10 times the number of moles of adamantane. A large amount of bromine will often cause environmental pollution, and it also needs to involve the process of recovering bromine, which is relatively complicated; secondly, adamantane bromide The hydrolysis reaction of alkane in water requires a long reaction time, which is not conducive to industrial production

Method used

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  • Method for preparing 1-adamantanol
  • Method for preparing 1-adamantanol
  • Method for preparing 1-adamantanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Such as figure 1 As shown, add 1.7g of 1-chloroadamantane into the preheater to vaporize, use an air pump to feed into the gaseous reactor, and feed water vapor at the same time, the reaction temperature is 160°C, and the reaction is 10s. Stop the reaction and cool to room temperature. The crude product of 1-adamantanol was obtained after filtration, and a sample was taken for GC analysis, and the conversion rate was 65.4%.

Embodiment 2

[0026] Such as figure 1 As shown, add 1.7g of 1-chloroadamantane into the preheater to vaporize, use an air pump to feed into the gaseous reactor, and feed water vapor at the same time, the reaction temperature is 160°C, and the reaction is 20s. Stop the reaction and cool to room temperature. The crude product of 1-adamantanol was obtained after filtration, and a sample was taken for GC analysis, and the conversion rate was 80.3%.

Embodiment 3

[0028] Such as figure 1 As shown, add 1.7g of 1-chloroadamantane into the preheater to vaporize, use an air pump to feed into the gaseous reactor, and feed water vapor at the same time, the reaction temperature is 170°C, and the reaction is 10s. Stop the reaction and cool to room temperature. The crude product of 1-adamantanol was obtained after filtration, and a sample was taken for GC analysis, and the conversion rate was 90.3%.

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Abstract

The invention relates to a method for preparing 1-adamantanol. The method is characterized in that 1-chloroadamantane and vapor react to obtain 1-adamantanol. According to the method, 1-chloroadamantane is taken as the raw material to synthesize 1-adamantanol, the reaction yield is high, the reaction time is short, only one-step operation is required, pollution is small, and a high implementation value is achieved.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 1-adamantanol. Background technique [0002] 1-Adamantanol is an important active intermediate for the synthesis of fine chemicals such as adamantane derivatives. It can be acylated, carboxylated, and esterified under certain conditions to generate a wide variety of adamantane derivatives, which are widely used In medicine, daily chemical, materials and other fields. [0003] Cohen and Keinar et al. (Kinetics of ozone.6.polycyclic aliphalichydrocarbons[J].J.Org.Chem.1988,53,3429) used silica gel as an ozone carrier, first mixed adamantane with silica gel, and then passed through at -75°C Adding ozone to saturation, and then slowly raising the temperature to room temperature, can obtain 1-adamantanol, the yield and conversion rate are both over 99%, and the product is pure without by-products such as 2-adamantanol. [0004] [0005] Mello R...

Claims

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Application Information

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IPC IPC(8): C07C29/124C07C35/37
Inventor 李士坤胡晓春孔黎春罗芳
Owner ZHEJIANG NORMAL UNIVERSITY
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