SU1342904A1 - Method of producing dactylin - Google Patents

Abstract

The invention relates to heterocyclic compounds, in particular to the preparation of dactilin (DC). The goal is to simplify the process, increase the output of DC and expand the resource base of the method. Getting DK lead extraction plant materials - air-dried flowers Astragalus galegiformis L 75-90% ethanol at boiling. The solvent is evaporated, the residue is crystallized from alcohol, followed by drying the product. The method provides an increase in the output of DK from 0.3 to 0.5% while reducing the number of operations from 12 to 6. e

Description

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Izs1G11i t (M1 does not refer to ss; ss; s to the callee ATP to receive dactylia (astragleguloid).

The lU Jib of the invention is a simplification of the technology, a strangle product release and an expansion of the raw material of the 1.1 method.

Example 1. Take 10 kg of air-dried crushed to C, 09 mm flowers of Astragalus galegiformis L. Extract ten times a day, 1m amount of 80% alcohol v: extractor when heated to 79., t C.

The obtained extracts are combined, distilled off under vacuum (residual pressure of 3 mm Hg), at 70 (; until complete removal of 1P5 alcohol. The resulting aqueous residue (10 l) is purified 3 l of chloroform 3 times. Olschonny) thus extract leave at room temperature until crystals precipitate. The crystals that precipitated out were collected by filtration and were recrystallized from 5 liters of alcohol. The alcoholic solution is concentrated and the crystals separated out are filtered off, washed with alcohol and dried at room temperature. This gives 49 grams of distillation (that is 0 with respect to the air-dry raw material. The process is carried out in 120 hours.

Example 2: 10 kg of air-dry seeds of Astra flowers (up to 0.09 mm) are given; alus ga 1 egi formts L. Extracted with ten times the amount of 75% alcohol in the extractor when heated to 74.5 C, then The process by CI11 process is carried out analogously to example 1. In this case, 39 IG of a product is obtained, which amounts to (1, 9% in terms of (air dry material).

Prim with p. Take 1 (1 kg air-dry and 1elch ml of up to 0.09 mm tsveksi - Ast HMG..H 1 us yes 1 f orinis L. Extract extra 14 and tick with 90% i-1 alcohol in the extractor with heat 78, (/. Then the process engineer named KI11 about the PS of its drying is analogous to (-py 1. 42.0 of the virra are produced, which is 0%, 42% for pt1); irish-dry

cheese .10.

 Noluchspm; IU) represents ciiOoi i I1-.1I nii.iv.i - -.py; 4 1 1 glycotic glycotic ;; -) 11-1-3, 4 -digly-CHI1, H, i) i.1: H H -: m i, i; uM O iiLh.M (lacti. pp-- I.

). 42

The individual dactylin is confirmed by the following physicochemical constants of the substance; m.p. 276-, MfUi.M. (spectrophotometric) L40, corresponding to the composition C, AND “O ,,.

in different solvent systems KDHetuihiA П11ДУКТ gives one non-soluble

jniMoe is plain. R. in the systems: n-butanol-uss, the kilo lot is water (4: 1: 2) 0.38; Pb-on acetic acid 0.41; ethyl acetate - formic acid - water (10: 2: 3) 0.10.

Displacement test: g; p1coside with a reliable sample of dactilin depression m.p. does not show.

In the quantitative hydrolysis of the product (formed arJuiKOH with the release of

48%, which indicates its biozidnuyu nature.

Quantitative content: the amount of dactilin in the final product is on average 96-98%.

PRI me R 4 (known). 50 g of crushed raw material is extracted in Soxhlet’s apparatus with chloroform (for i h), the material is dried in air, and again extracted with 95% alcohol

within 24 hours. The alcoholic extract is evaporated until an oily mass is obtained, 25 nd ace 1-one is added to this mass, the solution is heated to boiling and cooled, decanted. This process is repeated three times. The resulting gum-like mass is dissolved in 10-15 ml of water with heating to boiling, pacTBcjp is filtered and cooled to 2 ° C over a period of several weeks. Wherein

the substance crystallized from the solution, KciTopoe was filtered off, washed with water. nd on the filter and dried. After a perekrist: .pizizatsii from the water produce crystals the same. yogogo color in quantity

150 mg (yield 0.3%), which is filtered, washed on the filter and dried.

In comparison with the known, the proposed method provides an increase in the yield of dactilin from 0.3 to 0.5%, and

Claims (1)

the number of operations is reduced from 12 to 6, the claims of the invention The method for producing dactilin by extracting vegetable raw materials with organic solvent at boiling, evaporation of the crystallization solvent and drying the product, in order to simplify .1 G- :. M (): 4 1 SRI ripcMiec sa, poiyshsii vmholl tso-mis L., 1chipt 51, gkstrl I ni vm i / - the horn of 1 product and expansion of raw materials - 902th these, 1: pirat-pm, and ii iiiytrn basis of the method, as a plant | iodine iodine clip iioi,:.: n. the pythonic raw materials use post-alcohol othigtsyt-chloro-chorm, and Fxpirc dry Astragalus galegifor-tallets; Lead from alcohol.