The method of receiving beaupreau

 

(57) Abstract:

The invention relates to a method for producing high molecular weight unsaturated alcohols of beaupreau, which are used for the production of biologically active substances and drugs. The method of receiving beaupreau General formula given in the text descriptions of unsaponifiable substances sulfate soap obtained in sulphate cooking hardwoods, a column of silica gel using as eluent a mixture of petroleum ether and diethyl ether. Chromatographic separation is carried out in the mode of gradient elution in the allocation of non-polar and monopolarly components and overload the column break - use front-enrichment. The proposed method allows one to obtain the pure drugs and increase the productivity of the process.

The invention relates to a method for producing high molecular weight unsaturated alcohols of beaupreau (polyprenols) with the number of carbon atoms of 30 to 45 and the number of isoprene units 6 - 9 of substances sulfate soap derived from hardwoods, which are used for obtaining biologically active substances of the ptx2">

1. Getting beaupreau of their chips birch tree [2] the chips are extracted with acetone for 24 hours, then the acetone evaporated. The residue is extracted with diethyl ether and evaporated to a syrup. The latter is treated with petroleum ether. The petroleum ether extract omelet potassium hydroxide in methanol solution and receive acidic and neutral fractions.

From the neutral fraction via chromatography on silica gel with a mixture of petroleum and diisopropyl ether in a ratio of 1:1 by volume secrete Betulaceae. Obtain 0.8 g of beaupreau of 9,34 g of extract in petroleum ether, which is 11.7% of the weight of the extract or 1% by weight of birch shavings.

2. Getting polyprenols from extracts of pine greenery with the number of carbon atoms of 65 to 90 and the number of isoprene units 12 - 18 [3]. Obtaining carried by the following methods: chromatography, fractional dissolution, fractional freezing, molecular distillation, or a combination of both. Because pine green polyprenols are present in the form of acetates (about 70 wt. %) and alcohols (about 30 wt.%), the authors use several techniques in the allocation of polyprenols: (a) saponification of the extract from IRow, including acetates polyprenols, saponification and separation on the second column of silica gel unsaponifiable substances. If the mass of the extract from green small for separation using thin layer chromatography (TLC) and liquid chromatography (elixir, KCC). For the separation of large quantities of extract used column chromatography using a variety of sorbents, preference is given to silica gel. As eluents used a mixture of nonpolar and polar solvents, taken in a wide range of relations. As follows from the examples, the elution mode - isocratic, i.e., a constant ratio of polar and non-polar component, without overloading the column break.

Example 1: the mass of sorbent 300 g sample weight 51 g (1.5% of the sample from the mass of sorbent).

Example 2: the mass of sorbent 100 g sample weight of 2.7 g (2.7% of the sample from the mass of sorbent).

The purity of the secreted product is not less than 90%. Control over the selection process is carried out by DSC and LC. The disadvantage of this method is a multistage and complexity that makes it difficult industrial implementation of the method.

The purpose of this method is to increase the performance of the process, the expansion of the materials is"ptx2">

This goal is achieved by a method of obtaining beaupreau General formula H-[CH2- C(CH3) = CH-CH2]n- OH, where n = 6 to 8, the processing of wood using chromatography. As wood use deciduous trees, which are subjected to a sulphate cooking, and any resulting unsaponifiables sulfate soap divided into chromatographic column with silicagel using as eluent a mixture of petroleum and diethyl ethers mode gradient elution with elution nonpolar and monopolarly components in the volumetric proportion of diethyl ether in eluent 5 - 8 wt. % and the elution of beaupreau when the volumetric proportion of diethyl ether in eluent 11 - 13 wt.% and the process when the overload column break, when you type in a column of unsaponifiable matter of 10 to 14 wt.% from the mass of sorbent.

As a source of raw material for beaupreau use unsaponifiables from sulfate soap, obtained by cooking hardwoods, and containing about 25% of beaupreau and unsaponifiables obtained after deposition of sterols and betulin and enriched Betulaceae (mass fraction of the latter about 40%) the purity 95 - 98%. The proposed method enables the regeneration column. It is performed in the following way. After separation of beaupreau other components of the mixture elute with a mixture of petroleum and diethyl ether, the volume past 50%. Then the column was washed with diethyl ether or isopropyl alcohol (one column volume) and petroleum ether (two volume of the column). The presence of impurities in Betulaceae controlled by TLC on plates type "Silufol", using as solvent a mixture of petroleum and diethyl ether, taken in equal relationships. Records show in iodine vapor. The value of Rfspots of beaupreau is 0.45 to 0.5.

Control over the purity of the fractions of beaupreau can be carried out by GLC (gas liquid chromatography) after transformation of polyprenols in primarilly esters in the column with a non-polar liquid phases such as SE - 30 column temperature of 250 - 280oC. the Method illustrated in the examples below.

Example 1. 15 g of unsaponifiable substances isolated from sulfate soap and containing 27% of beaupreau, was dissolved in 50 cm3petroleum ether and transferred to a column of silica gel (column length 30 cm, inner diameter is Talanova and diethyl ether (5 and 10% diethyl ether in petroleum). The amount of solvent in the allocation of each fraction was 200 cm3. Betulaceae allocate, passing through a column of 400 cm3the mixture petroliana and diethyl esters of the following composition: 88% petroleum ether and 12% diethyl ether. After removal of the solvent selected 3, 4 g of beaupreau, which is 22.7% of the original raw materials (84% of the original prenolol). Mass fraction of beaupreau in selected fractions according to GC is 95%. Analysis was performed by GLC column in SE - 30 at a temperature of 270oC. Betulaceae analyzed as trimethylsilyl ethers.

Example 2. 10 g "betulapendula" fractions containing 40% of beaupreau C6-C9, dissolved in 50 cm3petroleum ether and transferred to a column of silica gel with a length of 30 cm and an inner diameter of 3 cm, weight of silica gel 100 g (silica gel L 100/250 μm, Chemerol 4P).

Nonpolar and Malopolskie mixture of the components (hydrocarbons, ketones, aldehydes, esters, oxides) elute with petroleum ether and mixtures of petroleum and diethyl ether with the content of the last 5 and 8%, respectively. The volume of eluent in the allocation of each fraction is 200 cm3. Betulaceae allocate, passing through a column of 400 cm3the s samples elute 200 cm3a mixture of 50% petroleum and 50% diethyl ether.

After removal of the solvent there was obtained 3.1 g of beaupreau, that is 31% of the feedstock and 77.5% of the original beaupreau. Analysis of beaupreau by TLC showed the absence of sterols and monopolarly components. Condition analysis: plate "Silufol" 1515 cm, solvent: a mixture containing 50% petroleum ether and 50% diethyl ether.

Analysis of the fraction by GLC showed the presence at a fraction of beaupreau and triterpene alcohols. Mass fraction of beaupreau is 95%.

Example 3. 30 g Betulapendula" fractions containing 40% of beaupreau, was dissolved in 60 cm3petroleum ether and transferred to a column of silica gel (length 35 cm, inner diameter 4 cm, weight 220 g silica gel). Nonpolar and Malopolskie components suirable petroleum ether and its mixtures with 5 and 10% diethyl ether. The volume of solvent for each faction 300 cm3. Betulaceae allocate, passing through a column of 600 cm3the solvent of the following composition: 87% petroleum ether and 13% diethyl ether. After removal of the solvent selected 9,72 g beaupreau (32.4% of the feedstock or 81% of the original Betulaceae).

6-C9is 97%.

The advantages of the proposed method: the proposed method allows one to obtain pure preparations (mass fraction of prenolol not less than 95%). The method allows to increase the productivity of the process, increasing the ratio of the sample-sorbent. Bench tests of the method in the laboratory.

The method of receiving beaupreau General formula

< / BR>
where n = 6 - 9,

timber processing using chromatography, characterized in that the quality of the wood used deciduous trees, which are subjected to a sulphate cooking, and any resulting unsaponifiables sulfate soap separated through column chromatography with silica gel using as eluent a mixture of petroleum and diethyl ethers mode gradient elution with elution nonpolar and monopolarly components in the volumetric proportion of diethyl ether in eluent 5% to 8% and the elution of beaupreau when the volumetric proportion of diethyl ether in eluent 11 - 13% and the carrying out of the process when the overload column breakdown when this is entered in column unsaponifiables of 10 to 14 wt.% from the mass of sorbent.

 

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