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Method for preparing 1-hydroxyl-dimethyl adamantane

A technology of dimethyladamantane and hydroxyl, which is applied in the direction of hydrolysis preparation, etc., can solve the problems that are not conducive to improving the yield, reducing the production cost, and the DDQ oxidant is expensive, so as to reduce the production cost, increase the yield and reduce the cost. Effect

Inactive Publication Date: 2008-10-29
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

This method has the following disadvantages: the DDQ oxidant is relatively expensive, and the product is separated and purified by column chromatography, which is not conducive to improving the yield and reducing production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Embodiment 1: mainly comprise the following steps:

[0009] 1. React 100g of 1,3-dimethyladamantane with 50g of bromine at 50°C for 7 hours, use water as the hydrolysis reagent, and recover bromine after the reaction to obtain 1-bromo-3,5-dimethyl Adamantane;

[0010] 2. React 1-bromo-3,5-dimethyladamantane with 100ml of water at 40°C for 7 hours, cool, suction filter and wash with water to obtain 65.0g of 1-hydroxy-3,5-dimethyladamantane.

[0011] The yield is 95.3%, and the product purity is 99.4%.

Embodiment 2

[0012] Embodiment 2: mainly comprise the following steps:

[0013] 1. React 100g of 1,3-dimethyladamantane with 50g of bromine at 60°C for 6 hours, use water as the hydrolysis reagent, and recover bromine after the reaction to obtain 1-bromo-3,5-dimethyl Adamantane;

[0014] 2. React 1-bromo-3,5-dimethyladamantane with 100ml of water at 50°C for 6 hours, cool, filter with suction, and wash with water to obtain 65.5g of 1-hydroxy-3,5-dimethyladamantane.

[0015] The yield is 95.2%, and the product purity is 99.3%.

Embodiment 3

[0016] Embodiment 3: mainly comprise the following steps:

[0017] 1. React 100g of 1,3-dimethyladamantane with 50g of bromine at 70°C for 5 hours, use water as the hydrolysis reagent, and recover bromine after the reaction to obtain 1-bromo-3,5-dimethyl Adamantane;

[0018] 2. React 1-bromo-3,5-dimethyladamantane with 100ml of water at 60°C for 5 hours, cool, filter with suction, and wash with water to obtain 66.0g of 1-hydroxy-3,5-dimethyladamantane.

[0019] The yield is 95.4%, and the product purity is 99.5%.

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PUM

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Abstract

The invention relates to a method for preparing 1-hydroxy-3,5-dimethyl adamantine. The method comprises the steps as follows: (1) reacting 1,3-dimethyl adamantine and bromine at 40-100 DEG C for 0.25-10 hours with water being hydrolytic reaction reagent, and recovering bromine when the reaction is finished to obtain 1-bromo-3,5-dimethyl adamantine; and (2) reacting 1-bromo-3,5-dimethyl adamantine with water at 50-100 DEG C for 1-10 hours, cooling, vacuum filtering, water washing and collecting to obtain the target product. The obtained product has a yield of 95% or higher and a purity of more than 99.0%. Compared with the prior art, the method has the advantages that expensive chemical reagents and a silica gel column chromatography are not adopted, thus facilitating reducing production cost and improving yield.

Description

technical field [0001] The invention relates to a preparation method of 1-hydroxyl-3,5-dimethyladamantane. Background technique [0002] 1-Hydroxy-3,5-dimethyladamantane is an important intermediate in the manufacture of adamantane drugs. Document J Chem Soc Perkin Trans I (2001, P3230-3231) reported that DDQ was used as an oxidant, and in CF 3 React in COOH solution to obtain a single 1-alcohol, and use column chromatography to separate and purify the product. This method has the following disadvantages: the DDQ oxidant is relatively expensive, and the product is separated and purified by column chromatography, which is not conducive to increasing the yield and reducing production costs. Contents of the invention [0003] The purpose of the present invention is to provide a preparation method of 1-hydroxyl-3,5-dimethyladamantane, which can overcome the deficiencies in the prior art. [0004] The present invention is achieved like this: it mainly comprises the following...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/37C07C29/09
Inventor 任洪发鲁立万响林纪业明瞿东方顾振东梁健富宁异真
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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