Crystal form of demethylenetetrahydroberberine hydrochloride and preparation method thereof
一种亚甲基四氢小檗碱、盐酸的技术，应用在有机化学方法、医药配方、含有效成分的医用配制品等方向，达到制备成本低、产品质量好、好稳定性的效果
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Embodiment 1
[0043] Example 1. Synthesis of desmethylenetetrahydroberberine hydrochloride crystal form A
[0044] Add 5 g of berberine hydrochloride to 50 ml of ethanol and stir, slowly add 0.5 g of sodium borohydride, react for 4 h, and receive tetrahydroberberine hydrochloride after the reaction is over. Tetrahydroberberine hydrochloride was added to Phloroglucinol-H 2 SO 4 Stir in the system to make it completely dissolved. Under the catalysis of phloroglucinol, the reaction time is 0.5h, and the methylene group is removed to obtain demethylenetetrahydroberberine hydrochloride. The obtained product was dissolved in water, recrystallized, filtered with suction, the filter cake was collected, and dried to obtain crystals of desmethylenetetrahydroberberine A hydrochloride, which were weighed and detected. The X-ray powder diffraction pattern of the obtained solid is as follows figure 1 , the DSC diagram is as shown in figure 2 , the infrared spectrum as image 3 , the thermogravimetr...
Embodiment 2
[0045] Example 2. Synthesis of desmethylenetetrahydroberberine hydrochloride crystal form B
[0046] Add 5 g of berberine hydrochloride to 50 ml of ethanol and stir, slowly add 0.5 g of sodium borohydride, and react for 4 h. After the reaction ends, the product, tetrahydroberberine hydrochloride, is obtained. Tetrahydroberberine hydrochloride was added to Phloroglucinol-H 2 SO 4 Stir in the system to make it completely dissolved. Under the catalysis of phloroglucinol, the reaction time is 0.5h, and the methylene group is removed to obtain demethylenetetrahydroberberine hydrochloride. The obtained product was dissolved in methanol, added with ethyl acetate, recrystallized, filtered with suction, and the filter cake was collected and dried to obtain crystals of desmethylenetetrahydroberberine B hydrochloride, which were weighed and detected. The X-ray powder diffraction pattern of the obtained solid is as follows Figure 5 , the DSC diagram is as shown in Image 6 , the infr...
Embodiment 3
[0047] Example 3. Synthesis of desmethylenetetrahydroberberine hydrochloride crystal form C
[0048] Add 5 g of berberine hydrochloride to 50 ml of ethanol and stir, slowly add 0.5 g of sodium borohydride, and react for 4 h. After the reaction ends, the product, tetrahydroberberine hydrochloride, is obtained. Tetrahydroberberine hydrochloride was added to Phloroglucinol-H 2 SO 4 Stir in the system to make it completely dissolved. Under the catalysis of phloroglucinol, the reaction time is 0.5h, and the methylene group is removed to obtain demethylenetetrahydroberberine hydrochloride. The obtained product was dissolved in ethanol, ethyl acetate was added, recrystallized at 4 degrees Celsius overnight, suction filtration, the filter cake was collected, dried, and crystals of desmethylenetetrahydroberberine hydrochloride C were obtained, which were weighed and detected. The X-ray powder diffraction pattern of the obtained solid is as follows Figure 9 , the DSC diagram is as s...
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