The allocation method betulinol

 

(57) Abstract:

The invention relates to the field of chemical processing of birch bark (outer layer of birch bark). Describes the allocation method Betulinol (loop-20(29)-ene-3), 28-diol) with high mass fractions of the basic substance by extraction of the bark of the high-boiling hydrocarbon solvent (e.g. white spirit), characterized in that the extract is treated with an aqueous concentrated solution of sodium hydroxide, separating the resulting precipitate of sodium derivatives of fatty and triterpene acids, tenido, flavonoids, and the solution is cooled, separate the precipitation of Betulinol and dried. Mass fraction of the main substances in Betulinol increases to 88-90% compared with 76% without treatment of the extract with alkali. After a single recrystallization from alcohol2-C4and their acetates obtained Betulinol with mass fractions of the basic substance 97-99,5%. To reduce energy costs as extractant use white spirit-mother liquor from a previous operation, and extraction in the processing of wet bark are in the mode of azeotropic drying. 2 C.p. f-crystals, 2 tab.

The invention relates to the field of chemical processing of biomass the wood is 0(29)-EN-(3B,28-diol) (1) Pyh triterpene alcohol C30H50O2lupanovo series.

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Betulinol, its derivative products chemical transformations possess biological activity, in particular, antiseptic, gastro - and hepatoprotective properties, anti-tumor activity and are, due to the availability of raw materials (bark) and ease of selection of great potential interest for the pharmaceutical industry.

The generally accepted method of allocation Betulinol bark is extracted with an organic solvent followed by recrystallization of the extractive substances of which the main component is Betulinol. As extractant tested aliphatic hydrocarbons and their chlorinated benzene, alcohols, C1-C4diethyl ether, acetone /1-3/. In principle, all solvents except petroleum ether, are suitable for this purpose.

Thoroughly the process of extracting Betulinol bark studied in the work /3/, where the method is most similar to that proposed. It is shown that when using a hydrocarbon solvent with a boiling point 150-185oC mass fraction of Betulinol in extractive substances is 71%, and in the sediment obtained in the OHL is obtained from hydrocarbon extract, with a mass fraction of Betulinol 76%, was subjected to recrystallization from azeotropic mixtures with water, isopropanol and 2-butanol were Betulinol with mass fractions of the main substance of 90-94%.

The aim of the invention is to obtain Betulinol with higher mass down with the basic substance with lower energy costs.

The essence of the method lies in the fact that the extraction of lead circulating white spirit the mother liquor from a previous operation), the extract is treated with alkali, separating the precipitate from the extract is cooled and last drawn at this Betulinol filtered off, dried and optionally recrystallized.

When recrystallization of Betulinol as solvents used azeotropic mixture ethanol-water, isopropanol-water and water-saturated n-butanol, Isobutanol, 2-butanol, ethyl-, propyl and butyl.

In the processing of wet bark extraction was carried out in the mode azeotropic drying by removal of water.

The proposed method extracts derived from birch bark, treated with an aqueous concentrated solution of sodium hydroxide, to convert present in extractive substances polyphenols (tanney, fastwrites, and thus to separate them from Betulinol. From spent alkaline extract immediately crystallizes Betulinol with mass fractions of the basic substance 87-95% instead of 76%, as in the prototype /3/.

When recrystallization of this Betulinol obtained Betulinol high purity, with mass fractions of the basic substance of 97.5-99.5% pure.

In the processing of wet bark (up to 33% Rel.) directly with flow plywood production extraction was carried out in the mode azeotropic drying by removal of water to raise the temperature of the extraction and, as a consequence, the solvent capacity of the solvent. Which increases, ceteris paribus, output Betulinol. And extraction are not a pure hydrocarbon solvent, with the exception of the first operation, and the mother liquor after separation from the cooled extract vykristallizovyvalas Betulinol. This prevents the operation of the regeneration of the solvent from the mother liquor and reduced energy costs.

Example (control). 30 g of crushed bark (fraction of 5-15 mm) is extracted with 360 ml of white spirit at a temperature of 150-155oC for 2 hours. The extract is drained from birch bark, cooled, separated by filtration fallen extractives is responsible.

Example 1. 30 g of crushed bark (fraction of 5-15 mm) extracted 2 hours 360 ml of white spirit of the mother liquor, after separation of Betulinol from the cooled extract from prior experience. Hot extract is drained from birch bark and treated with 4 ml of 20% sodium hydroxide solution. The formed precipitate was separated from the hot extract. The extract is cooled to ambient temperature, the precipitated crystalline precipitate of Betulinol filtered off and dried. The output of 14.3% from the abs.dry.bark, mass fraction of the main substances and 88.8%. In a parallel experience: 13,3 and 89.1%, respectively.

In table.1 shows examples for obtaining Betulinol according to the recipe of example 1 by treatment with alkali, but in the different extraction conditions (duration, degree of grinding bark, and so on).

From the above examples it is seen that the output Betulinol depends on the duration of the extraction, the ratio of bark : the extractant, but in all cases, regardless of the degree of extraction of extractive substances in the processing of the extract lye on the proposed method obtained Betulinol with higher mass fractions of the basic substance - 87-95%, instead 73,0-76,0% in the control sample without treatment with alkali.

To obtain betonirakenteet from different solvents. For recrystallization, used a mixture of water-soluble alcohols with water azeotropic composition corresponding to the pressure, which is the distillation of the solvent in its regeneration and water-saturated solvent: butanol-1, butanol-2, Isobutanol, ethyl-, propyl - and butyl. The results of experiments on the use of such solvents are given in table. 2. The use of azeotropic mixtures not only increases the selectivity of crystallization, but also reduces the energy consumption at the stage of regeneration of solvents.

From table. 2 shows that when the recrystallization is obtained Betulinol with high mass fractions of the basic substance of 97.5-99.5% pure.

The method developed in the laboratory, the implementation of it will not be difficult due to the simplicity of technological operations.

Sources of information

1. Pasich /Emulgatory z grupy t th j Ferpenoidau c. 1. Ekstrakcja betuliny z kory brozoney Betula alba Z. za Pomoca trojchlozetilencu // Fannac polska - 1964 - Bd 20, N 23-24, S. 911-914.

2. Jaaskelainen P. Betulinol and its utilization // Paperi ja Puu - Pap. och. Fra - 1981. - N 10. - P. 599-603.

3. Eckerman Ch. , Ekman R. Comparison of solvents for extraction and crystallisation of betulind arom bisch bark Waste // Paperi ja Puu. och Tra - 1985. - N 3. - P. 100-106 (prototipo).

4. Chernyaev, N., Dolgopolova S. I. Degree R. D. Recycling of wood Bia organic solvents, characterized in that the extraction of lead circulating white spirit-mother liquor from a previous operation), the extract is treated with alkali, separating the precipitate from the extract is cooled and last drawn at this Betulinol filtered off, dried and optionally recrystallized.

2. The method according to p. 1, characterized in that during recrystallization of Betulinol as solvents used azeotropic mixture ethanol-water, isopropanol-water and water-saturated n-butanol, Isobutanol, 2-butanol, ethyl-, propyl - and butyl.

3. The method according to p. 1, characterized in that in the processing of wet bark extraction was carried out in the mode azeotropic drying by removal of water.

 

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11 cl, 1 tbl, 9 ex

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