Levobupivacaine hydrochloride crystal form A and preparation method thereof
A technology of levobupivacaine hydrochloride and crystal form, which is applied in the field of pharmaceutical preparation and achieves the effect of good performance and favorable transfer
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Embodiment 1
[0020] Add 900mL of methyl ethyl ketone and 900mL of ethyl acetate into a 3L reaction kettle, add 300g of levobupivacaine hydrochloride crude product under stirring, and heat to 100g; ℃ and filtered it into another 3L reaction kettle while it was hot, cooled to 20 ℃ for 2.5 hours to crystallize, and then cooled to 0 ℃ for 6 hours to crystallize. After the crystallization was completed, a white solid was obtained by filtration, and then dried at 60° C. for 6 hours. Determined by X-powder diffraction, see figure 1 , the reflection angle 2θ has characteristic peaks at about 9.6786, 10.6164, 12.5864, 13.3324, 18.9888, 21.5685; detected by infrared absorption spectrum, see figure 2 , at 3103.46, 2875.86, 1674.21, 1537.27, 1473.62, 786.96cm -1 .
Embodiment 2
[0022] Add 2.1L of methyl ethyl ketone and 2.3L of ethyl acetate into a 5L reaction kettle, add 700g of levobupivacaine hydrochloride crude product under stirring, and heat to 80°C; after refluxing and dissolving, add 35g of silica gel and continue stirring for 1 hour; At 60°C-70°C, filter while hot into another 5L reactor, cool down to 20°C for crystallization for 2.5 hours, then cool down to 0°C for 6 hours for crystallization. After the crystallization was completed, a white solid was obtained by filtration, and then dried at 55° C. for 6 hours. Determined by X-powder diffraction, see image 3 , the reflection angle 2θ has characteristic peaks at about 9.7177, 10.6572, 12.6361, 13.3865, 19.0401, 21.6302; detected by infrared spectroscopy, see Figure 4 , at 3101.54, 2877, 79, 1674.21, 1539.20, 1473.62, 786.96cm -1 .
Embodiment 3
[0024] Add 2.7L of methyl ethyl ketone and 3L of ethyl acetate into a 10L reaction kettle, add 1000g of levobupivacaine hydrochloride crude product under stirring, and heat to 77°C; ℃~70℃, filtered while hot into another 10L reactor, cooled to 20℃ for crystallization for 2.5 hours, and then cooled to 0℃ for 6 hours for crystallization. After the crystallization was completed, a white solid was obtained by filtration, and then dried at 62° C. for 6 hours. Determined by X-powder diffraction, see Figure 5 , the reflection angle 2θ has characteristic peaks at about 9.7355, 10.6925, 12.6543, 13.4132, 19.0551, 21.6469; detected by infrared spectroscopy, see Figure 6 , at 3103.46, 2875.86, 1674.21, 1537.27, 1473.62, 786.96cm -1 .
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