Meloxicam compound and purifying method thereof
A kind of technology of meloxicam and purification method, which is applied in the field of medicine and can solve the problems such as the inability to substantially improve the purity
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Embodiment 1
[0024] Dissolve 7g of meloxicam crude product (97.7% purity) in 300ml of dichloromethane-methanol (91:9) and add it to the top of the column. Silica gel. The length of the column is 20cm, the diameter is 3cm, the column pressure is 0.1pa, and then pumped into dichloromethane-methanol (91:9) for column chromatography, the flow rate is 0.5cm / min, the column temperature is kept at 30°C, start timing, sampling, and follow-up monitoring , collected in sections, collected the liquid, washed with water, dried over anhydrous sodium sulfate, concentrated under reduced pressure, and evaporated the eluent to obtain 6.5 g of meloxicam purified product, with a yield of 92.8%, a melting point of 247°C, and a purity of 99.9%. .
Embodiment 2
[0026] Dissolve 28g of meloxicam crude product (purity: 97.3%) in 800ml of dichloromethane-methanol (95:5) and add it to the top of the column. Silica gel. The length of the column is 20cm, the diameter is 3cm, the column pressure is 4.0pa, and then pumped into dichloromethane-methanol (95:5) for column chromatography, the flow rate is 1.5cm / min, the column temperature is kept at 40°C, start timing, sampling, and follow-up monitoring , collected in sections, collected the liquid, washed with water, dried over anhydrous magnesium sulfate, concentrated under reduced pressure, and evaporated the eluent to obtain 26.1 g of meloxicam purified product, with a yield of 93.2%, a melting point of 248°C, and a purity of 99.8% .
Embodiment 3
[0028] Dissolve 15g of meloxicam crude product (98.0% purity) in 500ml of dichloromethane-methanol (99.9:0.1) and add it to the top of the column. Silica gel. The length of the column is 20cm, the diameter is 3cm, the column pressure is 1.5pa, and then pumped into dichloromethane-methanol (99.9:0.1) for column chromatography, the flow rate is 1.0cm / min, the column temperature is kept at 35°C, start timing, sampling, and follow-up monitoring , collected in sections, collected the liquid, washed with water, dried over activated alumina, concentrated under reduced pressure, and evaporated the eluent to obtain 13.7 g of purified meloxicam, with a yield of 91.3%, a melting point of 246°C, and a purity of 99.9%.
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