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Method for preparing anti-para amino adamantanol

A technology of aminoadamantanol and trans, which is applied in the field of preparation of trans-aminoadamantanol, can solve problems such as poor effect, and achieve the effect of high conversion rate and simple process

Inactive Publication Date: 2011-07-20
上海博康精细化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Preparation of trans-p-aminoadamantanol Hydrolysis of 42 isopropyliminoadamantanol to prepare trans-p-aminoadamantanol took some troubles in the selection of hydrolyzing agent, mainly selected some acidic reagents as hydrolyzing agent, and the experiment proved the effect Bad, such as boric acid, acid diatomaceous earth, hydrochloric acid, sulfuric acid, the hydrolysis rate varies from 10% to 30%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation method for trans-aminoadamantanol, the method comprising the following steps:

[0020] (1) Preparation of trans-aminoadamantanol crude product: Dissolve 41.2g of p-aminoadamantanol in 200ml of glacial acetic acid, heat up to 65°C until p-aminoadamantanol is completely dissolved, and after the reaction system is clarified, use constant Add 66.6ml (about 0.7mol) of acetic anhydride to the pressure dropping funnel at a constant speed, continue to heat up to 80°C, and react at a constant temperature for 2 hours. Distill the resulting reaction solution under reduced pressure to remove glacial acetic acid and excess acetic anhydride, and then add distilled water for 5 times. , 10mL each time, then drain until a large amount of white powdery solids appear, then add 100ml of acetone, reflux to dissolve, cool and crystallize to obtain a filter cake, filter the filter cake with suction and wash with a small amount of acetone, and distill the filtrate under reduced pr...

Embodiment 2

[0024] A preparation method for trans-aminoadamantanol, the method comprising the following steps:

[0025] (1) Preparation of trans-aminoadamantanol crude product: Dissolve 40g of p-aminoadamantanol in 200g of glacial acetic acid (190ml), heat up to 60°C until the p-aminoadamantanol is completely dissolved, and after the reaction system is clarified, Use a constant pressure dropping funnel to add 57ml of acetic anhydride dropwise at a constant speed, continue to heat up to 75°C, and react at a constant temperature for 2 hours. The resulting reaction solution is subjected to vacuum distillation to remove glacial acetic acid and excess acetic anhydride, and distilled water is added 4 times, each time 10mL , and then drained until a large amount of white powdery solids appeared, then added 95ml of acetone, refluxed to dissolve, cooled and crystallized to obtain a filter cake, suction filtered the filter cake and washed with a small amount of acetone, and then dried the filter cak...

Embodiment 3

[0029] A preparation method for trans-aminoadamantanol, the method comprising the following steps:

[0030] (1) Preparation of trans-aminoadamantanol crude product: Dissolve 40g of p-aminoadamantanol in 220g of glacial acetic acid (210ml), heat up to 65°C until the p-aminoadamantanol is completely dissolved, and after the reaction system is clarified, Use a constant pressure dropping funnel to add 74ml of acetic anhydride dropwise at a constant speed, continue to heat up to 80°C, and react at a constant temperature for 3 hours. Distill the resulting reaction solution under reduced pressure to remove glacial acetic acid and excess acetic anhydride, and add distilled water 5 times, 10mL each time , and then drained until a large amount of white powdery solids appeared, then added 105ml of acetone, refluxed to dissolve, cooled and crystallized to obtain a filter cake, suction filtered the filter cake and washed with a small amount of acetone, and then dried the filter cake to obta...

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PUM

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Abstract

The invention relates to a method for preparing anti-para amino adamantanol. The method comprises the following steps of: (1) preparing a crude anti-para amino adamantanol product; (2) extracting pig kidney amino-acylase; and (3) resolving amino adamantanol so as to obtain the anti-para amino adamantanol with higher purity. Compared with the prior art, the method has the advantages that: racemic para amino adamantanol is successfully dissolved by using the pig kidney amino-acylase for the first time, so that the anti-para amino adamantanol is obtained; the method has a simple process and a high conversion rate; and the maximum yield can reach 71.8 percent.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of trans-aminoadamantanol. Background technique [0002] Trans-para-aminoadamantanol is an intermediate in the synthesis of anti-AIDS drugs. The reported synthetic route is to separate cis-trans-trans-acetamidoadamantanol by crystallization or column separation, and the total reaction yield is 27%. [0003] Preparation of trans-p-aminoadamantanol Hydrolysis of 42 isopropyliminoadamantanol to prepare trans-p-aminoadamantanol took some troubles in the selection of hydrolyzing agent, mainly selected some acidic reagents as hydrolyzing agent, and the experiment proved the effect Bad, such as boric acid, acidic diatomaceous earth, hydrochloric acid, sulfuric acid, the hydrolysis rate varies from 10% to 30%. Finally, good experimental results can be obtained by hydrolysis with sodium hydroxide. The hydrolysis rate is 98%-99%. The mother liqu...

Claims

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Application Information

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IPC IPC(8): C12P41/00C12P15/00
Inventor 傅志伟
Owner 上海博康精细化工有限公司