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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.

Inactive Publication Date: 2006-06-14
山东山大康诺制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently marketed dosage forms include norcantharidin tablets and sodium norcantharidinate injection, both of which use the raw material of norcantharidin to prepare tablets and injections. At present, there is no preparation method, structure determination and Reports and patent documents on the preparation of water injection, powder injection and large infusion by using sodium norcantharidate simple substance

Method used

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  • Demethyl sodium cartharidate medicinal compound and its preparation method and application
  • Demethyl sodium cartharidate medicinal compound and its preparation method and application
  • Demethyl sodium cartharidate medicinal compound and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: norcantharidate sodium synthesis

[0019] At room temperature, norcantharidin (100g, 0.60mol) and sodium hydroxide (47.6g, 1.20mol) are added in the reaction flask, water (300ml) is added, and the stirring reaction is no longer changed until the pH is added, and activated carbon for needles ( 1.5 g), stirred for 30 minutes, filtered, the filtrate was evaporated to dryness at 120°C, and dried in vacuum at 80°C to obtain 135g of the product, with a yield of 98.5%.

[0020] Appearance: off-white crystalline powder

[0021] Content: 100%

[0022] HPLC method: chromatographic column is YWG-C 18 (5μm, 4.6mm×250mm), the mobile phase is 0.025mol L -1 Potassium dihydrogen phosphate solution-methanol (75:25) (pH3.0), the 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...

Embodiment 2

[0029] Embodiment 2: norcantharidate sodium synthesis

[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 does not change, add activated carbon for needles (1.5g), stirred for 30 minutes, filtered, the filtrate was evaporated to dryness at 140°C, and vacuum-dried at 80°C to obtain 136g of the product, with a yield of 99.2%.

[0031] Appearance: off-white crystalline powder

[0032] Content: 100%

[0033] HPLC method: chromatographic column is YWG-C 18 (5μm, 4.6mm×250mm), the mobile phase is 0.025mol L -1 Potassium dihydrogen phosphate solution-methanol (75:25) (pH3.0), the 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....

Embodiment 3

[0037] Embodiment 3: preparation of sodium norcantharidate injection

[0038] Prescription: Sodium Norcantharidate 13.7g

[0039] Add water for injection to 2000ml

[0040] Made 1000 pieces

[0041] Preparation:

[0042] (1) The ampoule is washed clean, dried and sterilized;

[0043] (2) Take by weighing norcantharidin sodium 13.7g, add prescription amount 90% water for injection, stir and dissolve;

[0044] (3) The medicinal liquid is adsorbed with 0.05% (w / v) medicinal charcoal for 30 minutes, and decarbonized and filtered;

[0045] (4) Add water for injection to the prescribed amount, and filter with a 0.22 μm microporous membrane;

[0046] (5) Inspection of intermediate products;

[0047] (6) Filling, 2ml each, melt-sealed;

[0048] (7) Sterilize with circulating steam at 100°C for 30 minutes;

[0049] (8) Full inspection.

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Abstract

The present invention discloses a disodium norcantharidinate medicine compound, its preparation method and application. Its molecular formula is C8H8O5Na2, and its molecular weight is 230.2. Said medicine is obtained by using 1 mol of norcantharidin and 2.0-2.5 mol of sodium hydroxide, making them be completely reacted at 2 deg.C-100deg.C, then making evaporation at 100deg.C-200deg.C to remove water content. Said invention also provides the application of said disodium norcantharidinate medicine compound in preparation of medicine for resisting tumor. It can be made into powder injection, liquid injection or transfusion preparation.

Description

technical field [0001] The invention relates to a medical compound of sodium norcantharidate; the invention also relates to a preparation method and application of the compound. Background technique [0002] Humans have used mylabris to treat diseases for more than 2,000 years. Mylabris is the dry body of the insects of the Coralaceae family Mylabris or the yellow and black Mylabris. It is said in "Wood Classics" that it is pungent, hot, and poisonous, and it returns to the liver, stomach, and kidneys. , large intestine and small intestine, has the effect of attacking toxins and eroding sores, removing stasis and dispelling stagnation. Cantharidin is the main active ingredient of cantharidin, which is mainly used in the treatment of liver cancer, esophageal cancer and gastric cancer. However, cantharidin has a strong stimulating effect on the urinary system, and its application is limited. Norcantharidin (norcantharidin) is a derivative of cantharidin. It is a new type of ...

Claims

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Application Information

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IPC IPC(8): C07D307/00A61K9/08A61K9/14A61K9/19A61K31/343A61P35/00
Inventor 赵桂森冯军涛李春民王小兵
Owner 山东山大康诺制药有限公司
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