The method of obtaining betulin

 

(57) Abstract:

The invention relates to a method of extraction of betulin from the outer layer of birch bark. The method is carried out by extraction of betulin extraction of shredded birch bark with a mixture of solvents containing tetralinyl ether 70-100oWith the addition of toluene from 30 to 75% of the total volume of the extractant, and then betulin crystallized. The yield of extract is from 16 to 25% of absolutely dry matter and the content of betulin from 90 to 95%. 1 table, 1 Il.

The invention relates to the field of chemistry and can be used for processing of birch bark is the outer layer of birch bark.

Large pulp and paper and wood processing enterprises in the inevitable bark of a birch wood annually accumulates a large quantity of bark. Birch bark is a valuable raw material for production of new biologically active substances. The main content of extractives from the bark is betulin. Betulin emit extraction with organic solvents and subsequent recrystallization. Betulin is used to treat a number of diseases, and also it is cheap starting compound for the synthesis of each is 992.06.16). The essence of the method lies in the fact that betulin derived from birch bark, pre-activated in conditions pisabarro of paratrechina with the following parameters: pressure 2-5 MPa, temperature 180-260oWith aging 60-360 C.

A method of obtaining betulin (RF Patent 2131882, C 07 J 53/00, 63/00, 1998.03.26). The method includes the activation of birch bark birch at a pressure of 2-5 MPa, a temperature of 180-260oSince that time 50-360 with, the treatment with alkali and extraction of the alcohol, while the activation of birch bark and its alkaline hydrolysis is carried out simultaneously with the alkali charge in the amount of 10-20% by weight of the absolutely dry bark.

The disadvantage of the above described methods of obtaining betulin is a relatively low yield of pure product.

The problem to which the invention is directed, is to increase output and improve the purity of betulin.

The problem is solved as follows.

The method of obtaining betulin-based extraction of betulin from birch bark by using a solvent and subsequent crystallization and is characterized by the fact that as a solvent, a mixture of solvents containing petroleum ether 70-100oAnd 30-75% toluene, is 90 to 95%.

The proposed method is illustrated by a drawing, which shows a flow chart of obtaining betulin.

Betulin extracted from birch bark by extraction with organic solvents and subsequent recrystallization. When used as a solvent hydrocarbon solvent with a boiling point 150-185oWith mass fraction of betulin and output extractives are at a high level.

For extraction take the outer layer of the bark of birch Betula Pendula Roth. Humidity bark (%) of absolutely dry raw material is not more than 5%. As a solvent, a mixture of solvents containing petroleum ether 70-100oWith (PE) and 30-75% toluene.

The technological process of extraction is as follows.

Shredded birch bark is loaded into the extractor 1, where collection 2 pump 3 serves solvent that is heated in the heater 4. Solvent vapours are condensed in the refrigerator 5. The duration of extraction 5 hours. After extraction of the hot extract is poured into the mold 6. Remaining solvent is distilled from the bark of live steam, the solvent is separated in Florentine 7 and enters the collector 2. The mold is equipped with a stirrer is CNY receiver 9 is evaporation in the evaporation apparatus 10. The solvent is removed from the precipitate acute ferry.

When using as a solvent a mixture containing petroleum ether 70-100oAnd 30-75% toluene, the extract yield is from 16 to 25% of absolutely dry matter and the content of betulin in sediments from 90 to 95%.

EXAMPLE 1.

For isolation of betulin from birch bark birch chose the method of extraction of the bark in the Soxhlet. The extraction was performed for three hours. For the extraction took the outer layer of the bark of birch Betula Pendula Roth. Bark (weight and weighing > 170 g) pre-crushed to particle sizes HH,1 mm Humidity of birch bark is 4.4% (determined by the method of drying the sample at a temperature of 105oC). As extractant was used a mixture of petroleum ether 70-100oWith 50% toluene in a ratio of 1:1 (volume 100 ml). The extract obtained was evaporated in a vacuum evaporator and dried at initial temperature 40oWith over calcium chloride CaCl2.

By extraction with a mixture of PE loloololol in the ratio of 1:1 betulin not crystallizes and precipitates upon cooling, and is easily filtered. The extract yield is 19.6% of absolutely dry matter. The method of column chromatography was primarily the extract is 5%. Output 33,3, So pl. 257-259oC.

EXAMPLE 2.

Obtaining betulin produced as in example 1.

As extractant was used a mixture of petroleum ether 70-100oWith 30% toluene.

The extract yield is 16.0% from absolutely dry matter. The content of betulin in the sediment is 91%. The content of lupeol, which is the main impurity in the extract, is 6%. The output of betulin 27,2, appearance - powder cream color, no mechanical impurities. So pl. 252-254oC.

The proposed method will be applied for obtaining betulin processing tonnage of waste produced during processing of birch.

The method of obtaining betulin extraction of betulin from birch bark by using a solvent, followed by crystallization, characterized in that as a solvent, a mixture of solvents containing petroleum ether 70-100oWith the addition of toluene from 30 to 75% of the total volume of the extractant.

 

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11 cl, 1 tbl, 9 ex

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