Urapidil hydrochloride crystal form and preparation method thereof
A technology of urapidil hydrochloride and crystal form, which is applied in the field of medicine and can solve problems such as the preparation of urapidil hydrochloride crystal form.
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Embodiment 1
[0055] The preparation of embodiment 1 urapidil hydrochloride crystal form
[0056] In a 250ml three-neck flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of refined urapidil, and heat to 60°C with stirring, but it cannot be clarified. Slowly add 3mol / L HCl / MeOH solution dropwise, so that the pH of the reaction solution is between 1-2 with a precision pH meter. At this time, the system is completely clear, continue to stir and keep warm for 1 hour, and slowly cool down to between 25-30°C , stirred at room temperature for about 2 hours, filtered, the filter cake was washed twice with 50ml of absolute ethanol, and the solid was dried in vacuo at 40°C to obtain 7.1g of product, yield: 89.6%, purity > 99% by HPLC, simplex < 0.05%, Product urapidil: HCl=1:1.12.
Embodiment 2
[0057] The preparation of embodiment 2 urapidil hydrochloride crystal form
[0058] In a 250ml three-neck flask equipped with a reflux condenser, add 160ml of absolute ethanol and 8.1g of refined urapidil, and heat to 60°C with stirring, but it cannot be clarified. Slowly add 3mol / L HCl / MeOH solution dropwise, so that the pH of the reaction solution is measured between 2-3 with a precision pH meter. At this time, the system is completely clear, continue to stir and keep warm for 1 hour, and slowly cool down to between 25-30°C , stirred at room temperature for about 2 hours, filtered, the filter cake was washed twice with 50ml of absolute ethanol, and the solid was dried in vacuo at 40°C to obtain 6.2g of product, yield: 75.8%, purity > 99% by HPLC, simplex < 0.05%, Product urapidil: HCl=1:1.2.
Embodiment 3
[0059] The preparation of embodiment 3 urapidil hydrochloride crystal form
[0060]In a 250ml three-neck flask equipped with a reflux condenser, add 165ml of absolute ethanol and 16.2g of refined urapidil, and heat to 60°C with stirring, but it cannot be clarified. Slowly add 3mol / L HCl / MeOH solution dropwise, so that the pH of the reaction solution is measured between 3-4 with a precision pH meter. At this time, the system is completely clear, continue to stir and keep warm for 1 hour, and slowly cool down to between 25-30°C , stirred at room temperature for about 2 hours, filtered, and the filter cake was washed twice with 50ml of absolute ethanol, and the solid was dried in vacuo at 40°C to obtain 15.6g of product, yield: 91.2%, purity > 99% by HPLC, simplex < 0.03%, Product urapidil: HCl=1:1.09.
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