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
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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 press
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 cake t
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 obtain
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