Preparation method of tilmicosin phosphate crystal
A technology for tilmicosin phosphate and crystals, which is applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of reducing the content of tilmicosin phosphate, bodily injury of operators, affecting normal use, and the like, To achieve the effect of reducing physical harm, reducing pollution, and fast dissolving
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Embodiment 1
[0021] Weigh 10 kg of tilmicosin phosphate powder, and measure 30 L of ethyl acetate. Add tilmicosin phosphate into ethyl acetate, start stirring to dissolve, and control the rotation speed at 20r / min. Then the temperature was lowered to 5° C., and isopropyl ether was slowly added in a state of stirring, and the amount of isopropyl ether added was 30 L. When adding dropwise, the amount added per minute is controlled to be 1 / 10 of the total amount, the rotational speed is controlled at 15 r / min, and the temperature is always controlled at 0-5°C throughout the process. After the dropwise addition, the stirring speed was controlled at 10r / min, and the stirring was continued for 1h. Use a centrifuge for solid-liquid separation. The solid obtained after centrifugation was washed twice with isopropyl ether at 5° C., the amount used for the first rinsing was 15 L, and the amount used for the second rinsing was 15 L. Under the temperature condition of 50°C, using a double-cone rota...
Embodiment 2
[0023] Weigh 10 kg of tilmicosin phosphate powder, and measure 40 L of ethyl acetate. Add tilmicosin phosphate into ethyl acetate, start stirring to dissolve, and control the rotation speed at 25r / min. Then lower the temperature to 3°C, slowly add isopropyl ether in a stirring state, the amount of isopropyl ether added is 60L, and the amount added per minute is controlled to be 1 / 10 of the total amount during the dropwise addition, and the speed is controlled at 25r / min. The temperature is always controlled at 0-5°C. After the dropwise addition, the stirring speed was controlled at 10r / min, and the stirring was continued for 1h. Solid-liquid separation using centrifuge equipment. The solid obtained after centrifugation was rinsed twice with isopropyl ether at 3° C., the first use amount was 29 L, and the second use amount was 30 L. Under the temperature condition of 55°C, using a double-cone rotary vacuum dryer, the vacuum degree was controlled at -0.05MPa, until the drying...
Embodiment 3
[0025] Weigh 10 kg of tilmicosin phosphate powder, and measure 50 L of ethyl acetate. Add tilmicosin phosphate into ethyl acetate, start stirring to dissolve, and control the rotation speed at 30r / min. Then lower the temperature to 0°C, slowly add isopropyl ether in a stirring state, the amount of isopropyl ether added is 100L, and the amount added per minute is controlled to be 1 / 10 of the total amount during the dropwise addition, and the speed is controlled at 30r / min. The temperature is always controlled at 0-5°C. After the dropwise addition, the stirring speed was controlled at 10r / min, and the stirring was continued for 1h. Solid-liquid separation using centrifuge equipment. The solid obtained after centrifugation was washed twice with isopropyl ether at 0° C., the amount of isopropyl ether used for the first time was 48 L, and the amount of isopropyl ether used for the second time was 49 L. Under the temperature condition of 60°C, a double-cone rotary vacuum dryer wa...
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