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Method for producing 1-adamantane ethanol

A technology of adamantanol and adamantane, which is applied in the field of high-purity 1-adamantanol products, and can solve problems such as difficult to meet the needs of downstream products, high manufacturing costs, and complicated post-processing

Inactive Publication Date: 2009-07-29
YIBIN CHEMIST PHARMACHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production of this product had incomplete bromination or excessive bromination before, resulting in poor product quality and complicated post-processing; the produced 1-adamantanol was of poor quality, low yield, high manufacturing cost, and it was difficult to meet the needs of downstream products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0006] Example 1: Synthesis of 1-bromoadamantane

[0007] Add 200kg of adamantane and 2kg of catalyst A into the clean and dry reaction kettle, and press 470kg of bromine into the upper tank. Slowly add bromine dropwise to the reaction kettle, and react at 60°C for 3 hours. After sampling and analysis are qualified, the bromine is recovered by distillation. The concentrated solution was added with dilute lye for neutralization, stirring and cooling were continued, and then the materials were centrifuged to obtain 318 kg of 1-bromoadamantane with a content of 98.5% and a yield of 99%.

Embodiment 2

[0008] Example 2: Synthesis of 1-adamantanol product

[0009] Add 350 kg of 1-bromoadamantane and 350 liters of water into the clean reaction kettle. The temperature is raised to 120° C., the pressure is 1.5 atm, and the hydrolysis reaction is conducted for 6 hours. Then the temperature is lowered, the product is precipitated, and the crude product of 1-adamantanol is obtained. After the crude product is decolorized and recrystallized, 238 kg of the refined product of 1-adamantanol is obtained, with a content of 99.7% and a yield of 97.4%.

Embodiment 3

[0010] Example 3: Synthesis of 1-adamantanol product

[0011] Add 350kg of 1-bromoadamantane and 350 liters of water into the clean reaction kettle, raise the temperature to 130°C, 2atm pressure, and hydrolyze for 5 hours. Then, the temperature is lowered and the product is precipitated to obtain crude 1-adamantanol. After the crude product is decolorized and recrystallized, 237 kg of refined 1-adamantanol is obtained, with a content of 99.6% and a yield of 96.9%.

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PUM

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Abstract

The invention relates to a method for producing a 1-adamantanol product which is prepared by subjecting adamantane to bromination reaction and hydrolysis reaction. Bromine is used as a halogenating agent, and the dosage is one to ten times of the adamantane in mole number. A is used as a bromination catalyst, and the dosage is 0.5 percent to 5 percent of the weight of the adamantane. The temperature of the bromination reaction is 0 DEG C to 100 DEG C, and the reaction pressure is normal pressure. The invention is characterized in that the hydrolysis temperature of 1-bromine adamantane is 100 DEG C to 150 DEG C, and the reaction pressure is 0-3atm. The purity of the 1-adamantanol obtained by the invention is more than or equal to 99.5 percent, and the yield is more than 95 percent.

Description

1. Technical Field [0001] The present invention relates to the production of 1-adamantanol products, and in particular provides a process of producing 1-adamantanol products by bromination and hydrolysis reaction of adamantane. 1-bromoadamantane is produced through catalytic bromination and under certain pressure. Method for producing low-cost and high-purity 1-adamantanol products under hydrolysis. 2. Background technology [0002] As an important fine chemical product, 1-adamantanol products have a wide range of applications in the fields of medicine, electronic materials and cosmetics. 1-adamantanol products are made from adamantane through bromination and hydrolysis. The production of this product had incomplete bromination or excessive bromination before, resulting in poor product quality and complicated post-processing; the produced 1-adamantanol had poor quality, low yield, and high manufacturing cost, and it was difficult to meet the needs of downstream products. [0003]...

Claims

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Application Information

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IPC IPC(8): C07C35/37C07C29/09
Inventor 谢运龙罗新平杨文广
Owner YIBIN CHEMIST PHARMACHEM CO LTD
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