A kind of oleanate and its preparation method and crystal
A technology of ethylenediamine salt and crystal of oleanolic acid, which is applied in the direction of steroidal compounds and organic chemistry, can solve the problems of strong hygroscopicity, low bioavailability, and poor water solubility of oleanolic acid salt, and achieve solubility and Good dissolution rate, high bioavailability, and low hygroscopicity
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Embodiment 1
[0032] The synthesis of ethylenediamine salt of oleanolic acid: put 100g (0.219mol) oleanolic acid into the reaction kettle, add 4L isopropanol, heat to dissolve at 75°C, add the isopropanol solution of ethylenediamine (ethylenediamine Amine 6.58g, namely 0.1095mol, isopropanol 0.408L), constant temperature, stirring at 100rpm for 2h, cooling down to room temperature at a cooling rate of 5°C / h, crystals precipitated, filtered, washed with isopropanol, and vacuum dried at 45°C for 24h. A white solid, ethylenediamine oleanolic acid, was obtained. The yield of ethylenediamine oleanolic acid was 87%.
Embodiment 2
[0034] The synthesis of ethylenediamine salt of oleanolic acid: 100g (0.219mol) oleanolic acid is put into the reaction kettle, add 4L water-saturated ethyl acetate, heat to dissolve at 75°C, add the ethyl acetate solution of ethylenediamine ( Ethylenediamine 6.58g, namely 0.1095mol, ethyl acetate 0.408L), constant temperature, stirring at 300rpm for 15min, cooling down to room temperature at a cooling rate of 2°C / h, crystals precipitated, filtered, washed with water-saturated ethyl acetate, vacuum at 45°C After drying for 24 hours, a white solid, ethylenediamine oleanolic acid, was obtained. The yield of ethylenediamine oleanolic acid was 91%. The obtained crystal particle size is 500 μm, and it is pulverized into 10 μm, 30 μm, 50 μm, 100 μm, 300 μm and other different particle size seeds with a ball mill, universal pulverizer, airflow pulverizer, hammer pulverizer or impact pulverizer for the following implementation Example use.
Embodiment 3
[0036] The synthesis of ethylenediamine salt of oleanolic acid: put 100g (0.219mol) oleanolic acid into the reaction kettle, add 4L isopropanol, heat to dissolve at 75°C, add the isopropanol solution of ethylenediamine (ethylenediamine Amine 6.58g (ie 0.1095mol, isopropanol 0.408L), constant temperature, stirring at 200rpm for 15min, cooling down to 45°C at a cooling rate of 5°C / h, adding seed crystals with a particle size of 10μm (0.1066g, uniformly suspended in In 100mL of water, the seed crystal accounts for 0.1% of the theoretical yield of oleanolic acid ethylenediamine salt), and the cooling rate is 5°C / h down to 4°C, crystals are precipitated, filtered, washed with isopropanol and dried in vacuum at 45°C for 24h , to obtain a white solid, that is, ethylenediamine oleanolic acid. The yield of ethylenediamine oleanolic acid was 89%.
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