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Method for preparing triptolide derivative

A technology of triptolide and derivatives, which is applied in the field of preparation of triptolide derivatives, can solve the problems of long time consumption and low efficiency, and achieve the effects of low preparation cost, high yield and easy availability of raw materials

Inactive Publication Date: 2012-08-08
FUJIAN ACAD OF MEDICAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Looking at various preparation methods, the physical method is the most classic method, but the disadvantage is that it takes a long time and is inefficient, and the extract is generally a mixture
Biological and chemical synthesis methods provide broad prospects for the large-scale preparation of active ingredients of Tripterygium wilfordii, but the corresponding preparation technology needs to be further improved

Method used

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preparation example Construction

[0013] The preparation method of triptolide derivative of the present invention, its technical scheme is as follows:

[0014] Dissolve 0.72-10.8g of triptolide in 70-1000ml of acetone, slowly add 10-150ml of tert-butanol dropwise, then add 0.18-2.7g of oxalic acid, 0.32-4.8g of iodine and 3-45g of iodine at room temperature Potassium thiocyanate, stirred at room temperature for 3 hours, after the reaction was completed, 80-1200ml of ethyl acetate was added to the reaction liquid for layering, the organic layer was washed three times with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and removed by distillation under reduced pressure Solvent, concentrate the residue on a 100-200 mesh neutral alumina column, elute with chloroform, collect the main fraction under TLC control, evaporate the solvent under reduced pressure, and recrystallize with acetone-ether to obtain white crystals, which is the Triptolide derivatives.

[0015] The...

Embodiment 1

[0017] First dissolve 2.4g (0.007mol) of triptolide in 230ml of acetone, slowly add dropwise 30ml of tert-butanol, add 0.6g (0.007mol) of oxalic acid, 1.07g of iodine (0.003mol) and 10g ( 0.1mol) potassium thiocyanate, stirred at room temperature for 3 hours, and the reaction was completed. 270ml of ethyl acetate was added to the reaction solution to separate the layers, the organic layer was washed twice with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and the solvent was distilled off under reduced pressure, and the residue was placed on a 100-200 mesh neutral alumina column. It was eluted with chloroform, and the main fraction was collected under TLC control (Rf: 0.38 (CHCL3 / MEOH 95:5), the chromogen was Kedd's reagent, which was purple). After distilling off the solvent under reduced pressure, recrystallize with acetone-ether (volume ratio: 10:1) to obtain 1.65 g of white crystals. Yield: 80%. The characterization data of...

Embodiment 2

[0021] First 10.8g (0.03mol) of triptolide was dissolved in 1000ml of acetone, 150ml of tert-butanol was slowly added dropwise, and 2.7g (0.03mol) of oxalic acid, 4.8g of iodine (0.015mol) and 45g ( 0.45mol) potassium thiocyanate, stirred at room temperature for 3 hours, and the reaction was completed. Add 1200ml of ethyl acetate to the reaction solution to separate the layers, wash the organic layer three times with saturated aqueous sodium chloride solution, dry over anhydrous magnesium sulfate, filter, distill off the solvent under reduced pressure, put the residue on a 100-200 mesh neutral alumina column, and use Chloroform was eluted, and the main fraction was collected under TLC control (CHCL3 / MEOH 95:5 was used as a developing solvent, and the chromogenic reagent was Kedd's reagent, which was purple). After distilling off the solvent under reduced pressure, it was recrystallized from acetone-diethyl ether to obtain 7.6 g of white crystals. The yield is 82%.

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Abstract

The invention provides a method for preparing a triptolide derivative, which comprises the following steps of: reacting triptolide used as a raw material respectively with tertiary butanol, oxalic acid, iodine and potassium rhodanide respectively at room temperature for 3 hours, separating, and then processing by using an aluminum peroxide column and recrystallizing to obtain the triptolide derivative. The invention has the advantages of no heating, short reaction time, easy easily obtained and low-cost material, simple and easy preparation method, low preparation cost, high yield and low isomer content and can be used to prepare effective component of Tripterygium wilfordii in a larger scale.

Description

technical field [0001] The invention relates to a preparation method of triptolide derivatives. Background technique [0002] Tripterygium wilfordii Hook.f. is a plant of the genus Tripterygium wilfordii Hook.f. There are 4 species in the world, 4 species are produced in China, and 3 species are used as medicine. Because Tripterygium wilfordii has significant physiological activities such as anti-inflammatory, immunosuppressive, anti-tumor, anti-cancer, and anti-fertility, it has been widely used in the treatment of rheumatism, skin disease, kidney disease and other diseases in the past 10 years; its immunosuppressive effect It has shown great application prospects in organ transplantation. But the toxicity of tripterygium wilfordii is very big, especially to liver, cardiovascular system, urinary system, reproductive system, digestive system and nervous system have very big toxic and side effects and mutagenic effect, poisoning death rate is as high as 29.6%, and these limi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J73/00
Inventor 郭舜民林绥朱惠阙慧卿
Owner FUJIAN ACAD OF MEDICAL SCI
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