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Method for preparing 1,3,7,9-tetramethyl uric acid

A technology of tetramethyluric acid and dichloromethane, applied in the field of chemistry, can solve the problems of difficult industrialized production, high solvent consumption and high process cost, and achieve the effects of simple operation, low solvent consumption and high purity

Active Publication Date: 2008-10-22
南京艾希帝生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the product of this invention has high purity, the bitter tea buds and leaves raw materials need to be steamed before the experiment, and finally separated by ODS column chromatography. The process cost is high, the steps are cumbersome, the solvent consumption is large and time-consuming, and it is also difficult to implement industrial production.

Method used

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  • Method for preparing 1,3,7,9-tetramethyl uric acid
  • Method for preparing 1,3,7,9-tetramethyl uric acid
  • Method for preparing 1,3,7,9-tetramethyl uric acid

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Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: adopt the wild bitter tea (Camellia assamica var.kucha) peel of Yunnan origin as raw material:

[0024] One, the preparation of bitter tea peel extract

[0025] Kucha fruit is collected from the wild Kucha tea tree in the place of origin in Yunnan Province. After drying, take out the seeds and crush the peel; weigh 1000g of bitter tea peel powder, add 10000mL of water to extract by ultrasonic (20kHz) at room temperature for 30min, and then heat Decoct for 1 hour, filter, add 8000 mL of water to the filter residue, heat and decoct for 1 hour, combine the two extracts, concentrate under reduced pressure to about 5000 mL, and obtain bitter tea peel extract.

[0026] Two, the preparation of 1,3,7,9-tetramethyluric acid crude product

[0027] The above extracts were extracted with 5000mL chloroform each time, and extracted 3 times in total, the chloroform extracts were combined, and the chloroform was recovered to dryness to obtain 17.2 g of light yellow powde...

Embodiment 2

[0039] Embodiment 2: adopt the wild bitter tea peel of the place of origin in Yunnan as raw material:

[0040] One, the preparation of bitter tea peel extract

[0041] Kucha fruit is collected from the wild Kucha tea tree in the place of origin in Yunnan Province. After drying, take out the seeds and crush the peel; weigh 100g of Kucha peel coarse powder, add 1500mL of water to extract by ultrasonic (80kHz) at room temperature for 10min, and then heat Decoct for 2 hours, filter, and concentrate the filtrate to 400 mL under reduced pressure to obtain bitter tea peel extract.

[0042] Two, the preparation of 1,3,7,9-tetramethyluric acid crude product

[0043] The above extract was extracted with 500 mL of dichloromethane each time, and extracted 3 times in total. The extracts were combined, and the dichloromethane was recovered to dryness to obtain 1.65 g of a light yellow powdery solid, of which 1, 3, 7, and 9 were measured by HPLC. - The content of tetramethyluric acid is 96...

Embodiment 3

[0046] Embodiment 3: adopt the cultivated Kucha pericarp of asexual cutting propagation in the tea garden of Sun Yat-sen University as raw material:

[0047] One, the preparation of bitter tea peel extract

[0048] After picking the Kucha fruit, take out the seeds after drying and crush the pericarp; weigh 100g of the Kucha pericarp powder, add 1000mL of water to extract by ultrasonic (40kHz) at room temperature for 30min, then heat and decoct for 1h, filter, and repeat the decoction for 2 hours. Once, the combined extracts were concentrated under reduced pressure to 500 mL to obtain Kucha pericarp extract.

[0049] Two, the preparation of 1,3,7,9-tetramethyluric acid crude product

[0050] The above extracts were extracted with 500ml of chloroform each time, and extracted twice in total, the chloroform extracts were combined, and the chloroform was recovered to dryness to obtain 1.45 g of light yellow powdery solids, of which 1,3,7,9-tetramethyl The content of base uric aci...

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Abstract

The invention discloses a preparation method for 1, 3, 7, 9-tetramethyluric acid, which relates to a preparation method for purine biology alkalies compound in the chemical field. Specifically, fruits of Camellia assamica var.kucha are used as raw materials, water is used for extraction, and the extracting solution is extracted from chloroform or dichloromethane; after the chloroform or dichloromethane is recycled, the ethanol solution with a volume percentage concentration of 50 to 100 percent or methanol is used as a solvent to be re-crystallized, and the 1, 3, 7, 9-tetramethyluric acid with 99 percent purity can be obtained. The preparation method for the 1, 3, 7, 9-tetramethyluric acid has the beneficial effects: 1. the preparation method has the advantage of waste utilization; 2. the preparation method with the advantages of simple technological process, little solvent usage, economy and time saving can realize industrialized production; 3. the product is high in purity and high in yield.

Description

technical field [0001] The invention relates to a preparation method of purine alkaloid compounds in the chemical field, in particular to a method for preparing 1,3,7,9-tetramethyluric acid from natural plants. Background technique [0002] 1,3,7,9-tetramethyluric acid (theacrine) belongs to purine alkaloids, and its structural formula is: [0003] [0004] The most well-known purine alkaloids in plants are three methyl derivatives of xanthine, namely caffeine (1,3,7-trimethylxanthine), theobromine (3,7-dimethylxanthine ) and theophylline (1,3-dimethylxanthine). Such substances have a wide range of physiological activities in the central nervous system, circulatory system, and respiratory system. [0005] Regarding the activity of 1,3,7,9-tetramethyluric acid, according to literature (Lyles MB, Cameron IL. Caffeine and other xanthines as cytochemical blockers and removers of heterocyclic DNA intercalators from chromatin, Cell Biol Int, 2002, 26: 145-154 ) report: 1,3,7...

Claims

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Application Information

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IPC IPC(8): C07D473/14A61P25/20A61K36/185
Inventor 王冬梅卢嘉丽叶创兴杜丽丽石祥刚郑新强
Owner 南京艾希帝生物科技有限公司
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