Method of purifying dapoxetine hydrochloride
A technology of dapoxetine hydrochloride and a purification method, which is applied in the field of medicinal chemistry, can solve the problems of low purity of dapoxetine hydrochloride, etc., and achieve the effects of easy control and industrial production, and high product purity
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Embodiment 1
[0040] Take 10g of dapoxetine hydrochloride crude drug (manufacturer Kebangte Chemical Co., Ltd., batch number 20140501) with a long production date, and the purity measured by high performance liquid chromatography is 94.48%. The dapoxetine hydrochloride raw material was dissolved in 40ml of acetone, fully stirred to make it completely dissolved, filtered to remove insoluble impurities, and the filtrate was collected once.
[0041] Add 0.2 g of activated carbon to the primary filtrate, stir and adsorb at 40°C for 15 minutes, filter the deactivated carbon, collect the secondary filtrate, and concentrate under reduced pressure at 60°C.
[0042] The secondary filtrate was heated to a temperature of 70-75°C and kept for half an hour, and then a mixed solvent of methanol and ethyl acetate (volume ratio 1:15) accounting for 300% of the solution volume was added. Cool down to 4°C at a rate of 5°C / hour. During this process, crystals slowly precipitate. After standing for 8-10 hours, ...
Embodiment 2
[0045] Take 10 g of expired dapoxetine hydrochloride crude drug (manufacturer Kebent Chemical Co., Ltd., batch number 20141201), and the purity measured by high performance liquid chromatography is 92.24%. Dissolve the dapoxetine hydrochloride raw material in 50ml of ethanol, stir fully to dissolve it completely, filter to remove insoluble impurities, and collect the filtrate once.
[0046] Add 0.3 g of activated carbon to the primary filtrate, stir and adsorb at 35°C for 10 minutes, filter the deactivated carbon, collect the secondary filtrate, and concentrate under reduced pressure at 55°C.
[0047] Heat the secondary filtrate to a temperature of 72-78°C and keep it for 1 hour, then add a mixed solvent of methanol and ethyl acetate (volume ratio 1:20) accounting for 300% of the solution volume, and lower the temperature at a rate of 5°C / hour At 0°C, crystals slowly precipitated during this process. After standing for 6 hours, the crystallization was complete, filtered, washe...
Embodiment 3
[0049] Take 10 g of crude dapoxetine hydrochloride prepared according to US5292962, and the purity is 93.28% as measured by high performance liquid chromatography. The dapoxetine hydrochloride raw material was dissolved in a mixed solvent of 60ml of ethanol and methanol, fully stirred to make it completely dissolved, filtered to remove insoluble impurities, and the filtrate was collected once.
[0050] Add 0.2 g of A-type molecular sieve to the primary filtrate, stir and adsorb at 35°C for 15 minutes, filter and remove the molecular sieve, collect the secondary filtrate, and concentrate under reduced pressure at 60°C.
[0051] Raise the temperature of the secondary filtrate to 70-75°C and keep it for half an hour, then add cyclohexane accounting for 300% of the solution volume, and cool down to 2°C at a rate of 5.5°C / hour, during which crystals slowly precipitate After standing for 8-12 hours, the crystallization was complete, centrifuged at 500 rpm, washed with a little water...
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