DD143261A1 - PROCESS FOR OBTAINING L - (+) ARABINOSE - Google Patents

Abstract

The invention has for its object to develop a cheap and industrially applicable method. According to the invention, sugar beet material is extracted with Viaser, then with water with the addition of Ca (OH), heated, filtered, the filtrate acidified with H2SO, J, hydrolysed by heating and

Description

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Inventor:. Tschiersch, Dr rer _{o o} nat.habil, Bruno Schwabe, Dr _{o o} reronat, Zonrad Stokov, Br.rer _o nat <,, Ilja

Process for the recovery of L - (+) arabinose

Field of application of the invention

The invention "relates to a process for the recovery of L - (- r) Aral in ο s e.

L - (+) Ara "biiiosis is used in microbiology, especially in bacteriology for diagnostic purposes, and serves as a starting material for chemical syntheses, including the synthesis of carcinostatic transport forms."

known _tik of "technical Solu tion s

In nature, L - (+) arabinose is widely used as the polysaccharide of higher plants, 'partly as a building block of the plant; lent en organisms, but partly also as a gummy Au ε £ cheiduzi ': £ Prodr; kt various "plant (acacia J, | ^i: | .sq.-üite-Grummi, cherry rubber and _{o e} a m.. ) _o

> Söhon in the older literature are described methods for the extraction of ...; Vpn L - (+) arabinose from plant materials ,, A;; summary gives S ₀ Harding (Sugar 24_, 656, 1922) ₀ . Generally, the plant materials are directly subjected to hydrolysis. Subsequently, L-arabinose is "isolated from the hydrolyzate." Also in more recent times, see, for example, B. So Anderson and L. Sands (Org. Synth., 1, 67, 1941), L (+) arabinous aas Mesquite gum is obtained by similar processes.The resulting product is due to varying amounts of impurities, which are always present in large quantities, and is produced only partially by other sugars, for subsequent synthetic work used, so that complex Heinigungsverfah- r s e äng se hl ο ss en he w d s s ss mu _β

: .y on'S. Harding (Sugar 2Λ_, 656, 1922) has also pointed out that sugar beets are a very good starting material for:; L - (+) arabinose production. "The same goes for Fo Janecek , F "Bendos and Y. Tibens-.icy; (CSSH Patent 153,378) 1975 described method, from the sugar beet or beet pulp L-arabinose, i3ectin and cellulose by hydrolysis with 0.1-6 % sulfuric acid won be "through the hydrolysis of the raw vegetative" materials, however, mixtures of sugars that only ^'arise;; very difficult splittable and therefore usually unclean, d "h". for further synthesis work hardly usable preparation pose.

Is also known from the literature that · from sugar beet pulp by heating with NaOH, the polysacchariä Araban solu- in "can be brought Sung _o From Ko Ka; (ji and _Φ β Tagavva b.BsA"

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207, 456, 1970) was used for induction Bo z _o of the enzyme L-oC-Arabinofüranosidase wherein the Aspergillus niger strain K ^

The authors carry out the extraction of the araban with NaOH solution and use the HCl-neutralized araban solution for the preparation of the healing media.

Object of the invention

The object of the invention is to develop a cheap and industrially applicable process for obtaining L - (+) arabinose.

Explanation of the essence of the invention

According to the invention, sugar beet material is extracted with cold or hot water to remove the sucrose and other water-soluble compounds. Subsequently, the plant material is mixed with 5-20 times, preferably 10 times the amount of water with the addition of 1-10 % (based on plant material), preferably 4 % Ca (OH) ₂ and for 10-120 minutes, preferably 30 minutes on 80-100 ° C, preferably 95 ⁰ C heated "Thereafter, the extract from the insoluble plant material and by adjusting to pH 3.0 is - formed CASOR 6.0 using sulfuric acid separated by filtration. By adding sulfuric acid, the H ₀ SO / - content of the extract is then brought to 0.2 - 3 % _t preferably 0.5 % and the araban contained in the solution then by heating to 80 100 C, preferably 95 ⁰ C within a period of 10 120 Minu t s, vo r to g sw else 60 Minu t s hydro Iy ε i t he _o major ch Z ugabe of Cacoo ^ sulfuric acid vird neutralized and the resulting CaSO ^ separated by subsequent filtration "the Piltrat contains, by thin-layer chromatographic analysis, L - (+) arabinone as the only sugar which is converted by concentration, crystallization or by extraction into a crystalline, pure product »

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Ausführungsbei game 1

100 g of sugar beet pellet material (information from the manufacturer: dry mass 890 g / kg, crude ash content 60 g / kg, total sugar content 650 g / kg) are heated 2 χ with 1000 ml of water to 95 ⁰ C and then filtered off _o so extracted plant material is added with 500 ml of water and 4 g of Ca (OH) ₂ and heated to 95 C for 30 minutes. After separation of the insoluble constituents by filtration, the araban-containing solution is brought to 0j5 Io HpSOr by addition of concentrated sulfuric acid and heated to 95 ° C for 60 minutes. The sulfuric acid is neutralized by treatment with CaCOo and then the resulting CaSO, separated by filtration. In the filtrate, L - (+) - arabinose is the only sugar detectable by thin layer chromatography. Bas FiI-trat is evaporated to dryness in vacuo at elevated temperature and the residue 4 χ with 200 ml of ethanol boiled The ethanolic extracts are used to separate dyes on a small AlpO-y column (ca _o 20 g AIpOo 'for the chromatography , Activity level 1, neutral). The AlpO column is washed with 600.ml ethanol. The combined sluates are strongly concentrated and the L - (+) arabinose is crystallized by standing at tree temperature. By cooling, the crystallization is completed.

Yield of pure L - (+) Arabinose: 4.2 g smpo: 145-150 ° (lit .: 159 ⁰ C)

Opt. Rotation: + 104 ° ^± 1 °, (c = 10 in H ₂ O); (Lit .: + 105 °) derivative: 1-Methyl-2,3,5-tri-O-benzcyl- U. -L-arabinofuranoside, mp .: 100 to 103.5 ⁰ C (Lit 100 .; 103 ⁰ C)

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Application example 2 ;

30 kg of sugar beet chips (moist) are placed in a 300 l-Zochgefäß and filled with water to 300 1 volume. It is boiled and then filtered through a plastic sieve. The ICoch process is repeated again. After re-filtration, the material is re-absorbed in water (300 1 final volume) and with 8 g of Ca (OH) ₂ /! added. The mixture is boiled for 1/2 h with stirring, filtered and the residue again with water (300 1 Er-dvolunen) for 5 min. Boiled Both filtrates are adjusted to pH 5 with 33% sulfuric acid and give a volume of 150 1, per 100 Flüssigkeit'werden 9 1 33 '% sulfuric acid is added and 6 hours at 8O ⁰ C heated by cooling is set by Cacoo to pH 5 the next day is decanted from the supernatant and the remainder on a Futsche sucked to 3TiItrat 2 kg Activated carbon (iTorit) / 100 1 given for decolorization. After filtration, the solution is concentrated in vacuo (4O ⁰ C) to a thick syrup. The syrup is added five times with five hot 99% ethanol and heated to 6O ⁰ C for 1 h. The alcohol extracts are thickened to syrup and this treated with 1 liter of 99% ethanol for about 1 hour begins the crystallization of L-arabinose, which is completed by keeping in the cold overnight. The product is finally washed on the filter twice with a little cold ethanol. Yield: 600 g L - (+) - arabinose ₀

Claims (2)

Inventions claim. 1. A process for obtaining L - (+) arabinose, which comprises extracting sugar beet material with water, then adding the plant material with 5-20 times the amount of water with the addition of 1-10 % (based on plant material) and for 10 - Heated to 80 100 C for 120 minutes, then the extract after adjustment 'to a pH 3.0 - 6.0, the. H ₂ S0.-content brings to 0.2-3 % and the araban contained in the solution by heating .80 - 100 ⁰ C within 10 _T. Hydrolyzed, neutralized and filtered for 120 minutes » 2. The method according to item 1, characterized in that preferably added with 4 % Ca (OH) ₂ , heated to 95 ° C for 30 minutes, the HpSO ^ content adjusted to 0.5 % and the hydrolysis at 95 C for 60 Minutes performed