Demethyl sodium cartharidate medicinal compound and its preparation method and application
A technology of sodium norcantharidate and a pharmaceutical compound is applied in the field of sodium norcantharidate pharmaceutical compound for medicine, and achieves the effects of convenient synthesis, huge application prospect and good water solubility.
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[0018] Example 1: Synthesis of sodium norcantharidinate
[0019] At room temperature, add norcantharidin (100g, 0.60mol) and sodium hydroxide (47.6g, 1.20mol) into the reaction flask, add water (300ml), stir the reaction until the pH does not change, add needle activated carbon ( 1.5g), stirred for 30 minutes, filtered, and the filtrate was evaporated to dry water at 120°C and dried in vacuum at 80°C to obtain 135g of product with a yield of 98.5%.
[0020] Properties: off-white crystalline powder
[0021] Content: 100%
[0022] HPLC method: chromatographic column is YWG-C 18 (5μm, 4.6mm×250mm), mobile phase is 0.025mol·L -1 Potassium dihydrogen phosphate solution-methanol (75:25) (pH3.0), detection wavelength is 210nm.
[0023] pH: 8.5 (10% aqueous solution)
[0024] IR(KBr)υ max : 2995, 2965, 2948, 2910, 1609, 1609, 1589, 1434, 1405.
[0025] 1 H-NMR(D 2 O)δ: 4.60 (s, H-13, H-16), 2.76 (s, H-14, H-15), 1.56 (m, H-10, H-12), 1.42 (m, H-9 , H-11).
[0026] 13 C-NMR(D 2 O)δ: 180.1(...
Example Embodiment
[0029] Example 2: Synthesis of sodium norcantharidinate
[0030] At 60°C, add norcantharidin (100g, 0.60mol) and sodium hydroxide (47.6g, 1.20mol) into the reaction flask, add water (300ml), stir the reaction until the pH no longer changes, add needle activated carbon (1.5g), stirred for 30 minutes, filtered, the filtrate was evaporated to dryness at 140°C, and dried under vacuum at 80°C to obtain 136g of product with a yield of 99.2%.
[0031] Properties: off-white crystalline powder
[0032] Content: 100%
[0033] HPLC method: chromatographic column is YWG-C 18 (5μm, 4.6mm×250mm), mobile phase is 0.025mol·L -1 Potassium dihydrogen phosphate solution-methanol (75:25) (pH3.0), detection wavelength is 210nm pH: 8.7 (10% aqueous solution) IR (KBr)υ max : 2998, 2970, 2945, 2911, 1610, 1585, 1430, 1408.
[0034] 1 H-NMR(D 2 O)δ: 4.60 (s, H-13, H-16), 2.76 (s, H-14, H-15), 1.56 (m, H-10, H-12), 1.42 (m, H-9 , H-11).
[0035] 13 C-NMR(D 2 O)δ: 180.1(C-7, C-8), 79.0(C-3, C-6), 55.1(C-4, ...
Example Embodiment
[0037] Example 3: Preparation of sodium norcantharidinate injection
[0038] Prescription: Sodium norcantharidinate 13.7g
[0039] Add water for injection to 2000ml
[0040] Made into 1000
[0041] Preparation:
[0042] (1) Wash the ampoule clean, dry and sterilize;
[0043] (2) Weigh 13.7 g of sodium norcantharidinate, add 90% of the prescription amount of water for injection, and stir to dissolve;
[0044] (3) The medicinal solution is adsorbed with 0.05% (w / v) medicinal charcoal for 30 minutes, and then decarburized and filtered;
[0045] (4) Add water for injection to the prescription amount and filter with 0.22μm microporous membrane;
[0046] (5) Intermediate product inspection;
[0047] (6) Filling, 2ml each, fusion sealing;
[0048] (7) Steam sterilization at 100°C for 30 minutes;
[0049] (8) Full inspection.
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