A kind of production technology of memantine hydrochloride
A technology of memantine hydrochloride and production process, applied in the field of medicine, can solve problems such as low final yield, and achieve the effects of avoiding the influence of yield, reducing side reactions and improving product yield
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Embodiment 1
[0030] Acetamidolation of 1-bromo-3,5-dimethyladamantane with acetonitrile under the action of concentrated sulfuric acid
[0031] The details are as follows: In a 500ml reaction flask, add 36.5g of 1-bromo-3,5-dimethyladamantane (0.15mol) and 105.75g of acetonitrile, then slowly add 280ml of concentrated sulfuric acid dropwise at a rate of 10-15 drops / minute (97%), stir. Control the reaction temperature at 5°C; stir at room temperature for 12 hours after dropping, then pour the reaction solution into ice water and let it stand for 10 hours, a white precipitate precipitates; filter with suction and dry the filter cake to obtain 1-acetylamino-3, The crude product of 5-dimethyladamantane was 32.49g, and the yield was 97.73%.
Embodiment 2
[0033] 1-Acetamido-3,5-dimethyl hydrolysis under basic conditions to give 1-amino-3,5-dimethyladamantane
[0034] The details are as follows: In a 500ml reaction flask, add 22.1g (0.1mol) of 1-acetylamino-3,5-dimethyladamantane prepared as described in Example 1, 20.1g of ethylene glycol, and 20g of hydrogen Sodium oxide and 55ml of water, slowly warm up and stir to dissolve the sodium hydroxide; control the temperature to 150°C and stir for 12 hours; stop stirring, cool the reaction solution to room temperature and transfer it to ice water, stir well, and let it stand for 1 hour. The oily matter precipitated; repeated extraction with 50ml of petroleum ether for 3 times, combined the petroleum ether layers for 3 times, dried the petroleum ether layer with anhydrous sodium sulfate, and then evaporated the petroleum ether to obtain a light yellow oily liquid which is 1-amino- 3,5-Dimethyladamantane.
Embodiment 3
[0036] 1-amino-3,5-dimethyladamantane was acidified to obtain memantine hydrochloride
[0037] Specifically as follows: get the oil prepared in Example 2, pass through dry hydrogen chloride, white solids are separated out, stop flowing hydrogen chloride gas when the solution pH=6, and the separated white solids are sucked and dried to obtain 19.93 g of memantine hydrochloride crude product, Yield 92.37% (Note: combined with the comprehensive yield of Examples 2 and 3).
[0038] Purification: recrystallized twice with chloroform to obtain 18.84g of the product, with a yield of 87.32% (note: combine the comprehensive yields of Examples 2 and 3).
[0039] For the memantine hydrochloride prepared in the continuous process of the above-mentioned examples 1-3, the comprehensive yield of the final product is 85.33%, which is far higher than the 79% yield of the final product of the memantine hydrochloride prepared in the prior art Chinese patent CN1335299A embodiment 1 . The produc...
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