A kind of preparation method of olmesartan medoxomil with low solvent residue
A technology of olmesartan medoxomil and low solvent residue, applied in the field of medicine, can solve problems such as easy residue, achieve the effect of reducing harm to human body and solving the problem of solvent residue
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Embodiment 1
[0030] 1) Take crude olmesartan medoxomil, use acetone to purify and crystallize (refer to CN102206208), and vacuum dry the olmesartan medoxomil after purification and crystallization for more than 3h under the conditions of ≤40°C and pressure ≥-0.08MPa, using a blast drying oven, The solvent residue of acetone was tested to be 0.4%.
[0031] 2) adding 1% absolute ethanol to the pre-dried olmesartan medoxomil, using a vibrating ultrafine pulverizer to pulverize, and pre-cooling the vibrating ultrafine pulverizer to -10°C to 0°C;
[0032] 3) Dry the pulverized olmesartan medoxomil for more than 2 hours in a vacuum drying oven under the conditions of ≤40°C and pressure >-0.08MPa.
[0033] Table 1 shows the comparison between the crushed particle size of olmesartan medoxomil and the acetone residue. Olmesartan medoxomil is pulverized to a particle size of D90=75μm or D90=60μm or D90=40μm or D90=20μm and then dried, and the acetone residues are all lower than the specified limit ...
Embodiment 2
[0037] 1) Take the crude olmesartan medoxomil, add acetonitrile with a mass ratio of 12 times the mass ratio of the crude olmesartan medoxomil, heat under reflux to dissolve, cool down to 0°C to 10°C after cooling and crystallization, and filter. The purified and crystallized olmesartan medoxomil was vacuum-dried for more than 4 hours using a rotary evaporator under the conditions of an inner temperature of ≤60° C. and a pressure of ≥-0.08 MPa, and the solvent residue of acetonitrile was detected to be 0.1%.
[0038] 2) Add 1.5% absolute ethanol to the pre-dried olmesartan medoxomil, pulverize with an airflow vortex micro-grinder, and cool the airflow vortex micro-grinder to -20-0°C in advance.
[0039] 3) Dry the pulverized olmesartan medoxomil at ≤60°C and normal pressure for more than 3 hours using a double cone.
[0040] The comparison relationship between the pulverized particle size of olmesartan medoxomil and the residual acetonitrile is shown in Table 2. Olmesartan me...
Embodiment 3
[0044] 1) Take the crude olmesartan medoxomil, add ethanol with a mass ratio of 13 times the crude olmesartan medoxomil, heat under reflux to dissolve, cool down to 0°C to 10°C after cooling and crystallization, and filter. The purified and crystallized olmesartan medoxomil was vacuum-dried for more than 4 hours in a vacuum drying oven at a temperature of ≤60° C. and a pressure of >-0.08 MPa, and the solvent residue of ethanol was detected to be 0.7%.
[0045] 2) Use a horizontal ball-milling ultra-fine pulverizer for pulverization, and pre-cool the horizontal ball-milling ultra-fine pulverizer to -10~0℃;
[0046] 3) Dry the pulverized olmesartan medoxomil at ≤60°C and normal pressure in a vacuum drying oven for more than 3 hours.
[0047] Table 3 shows the comparison between the crushed particle size of olmesartan medoxomil and the residual ethanol. Olmesartan medoxomil is pulverized to a particle size of D90=75μm or D90=60μm or D90=40μm or D90=20μm and then dried. The ethan...
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