SU672264A1 - Method of obtaining methyl esters of pynosylvine - Google Patents

Description

(54) METHOD FOR PREPARING METHYL ESTERS OF PINOSILVINE

The resulting npoflyitTfistalpizukug is initially ganol, and the sapiens are heptaine, the crystalline portions are removed, the non-crystallized part is processed by a wrench of Gerard, with the separation of carbonyl compounds and by the section and by the section, by a section, by a section, by a section, by a unit, by a section, by a section, by a unit, by a section, by a section, by a section, by a unit, by a section, by a unit, by a section, by a unit, by a unit, by a unit, by a section, by a unit, by a unit and by a section;

siyikagele. 6, petroleum vfir, benzene, or a mixture of petroleum ether and benzene, are used as a solvent. The fraction containing the target product in a quantity of 5.7% of the neutral substances of sulphate soap is injected with benzene.

This method is rather laborious. Due to its multiple UHfiHocifa, it allows to isolate only dimethyl ether of pinosylvin, which has insufficient bactericidal action, with a low yield.

The purpose of the invention is to simplify the gyogcophoid process and increase the yield of the target product.

The goal is achieved by the fact that. in the process for the production of methyl hydrophobicides, including the extraction of organic sulfate-cellulose by-product byproducts; solvents, separation and washing {1bp; Chenne, extract successively with water and water, distilling off the solvent and isolating the target product by chromatography of the residue, according to the invention, as a by-product; use black sulphate liquor, and,

chromatography of the residue was carried out by IMoHpHc W ftoeneShShSh tep. . . ,,

As an organic solvent, hexane, benzene, divtile wax, non-track can be used.

in $ yr or. of their mixture. . : .........

Example 1. 10 liters of black liquor get tip.H. brewing the hyperion cedar sulphate method

11 |) conditions of operation: consumption of aspivative M 1S, S% of the weight of the distillates, sulphidity of liquor 25%, rise time to 17O-17 C for 2 hours, cooking time at 8TH temperature for 2 hours.

The obtained EC block was cooled and extracted with three volumes of diviphen ether, the extract was washed with a 5% aqueous KOH solution, then with water, the solvent was distilled off. The obtained neutral substances (12 g). Chromatogra-

chromatographic chromatography

672264

fies on silica gel .. Elution was carried out first with hexane (500 ctf}, and then with mixtures of Hexane-divtil vfir (2%) 500 cm. This fraction (2% of the neutral substances) is 82% composed of the formula of dyhydrodimethyl vfira pinosylvin.

HgCOJAH 5H2

- V

the fraction eluted with 800 cm of hexane with the addition of 8% diethyl ether (10% of neutral substances), 93% ((X) consists of dimethyl vphyl zincsylvin. Yrie stored from the fraction eluted, crystals (melting point 5 2-54 ° C) .v

Fragae (13% of neutral substances), vplivae. The columns of hexane – divtile vfir are 1: 1 (500 cm) t at $ 8% cOtiTOtiT from a dihydromonomethyl e {}) ir range of pinosylvin and mono-methyl vfnr pinosylvin in the ratio, 5. Additional purification of the VTO and fractions of 5102 or AgN Oj. Pure DyHydromomonometil vfi monoMetylevir was isolated. pinosylvin (melting point 120–122 ° C). ,

The structure of isolated picosilvic monomers and dimethyl wyfirs, pinosylvin dihydromonomethyl ether and an IR, 5IMP, UV spectra with hardwires, and correspondingly light sources. The structure of dimethyl vfira is pyroscopic in the VGGDönayE spectral characteristics and iodine by chemical methods. -; .

PRI mme R 2. 16 g of neutral substances isolated as described in example I, out of 10 l of sulphate liquor obtained by cooking wood chips, {ntJS & itve & tHs under the conditions of example 1, are rotographed using column romatography. A mixture of petroleum and divine oil is used as a force.

Fractions (12% of neutral substances) are controlled by a mixture of petrose. Vyfir - divtil Vfire 1; 1, contains 92% Myyomyo pinosylvin sulphate.

Repeated chromatography of the fractions isolated individual monomethyl firm pinosylvin. (6.5% of neutral substances, melting point 5254 C) and dimetypical wines PINE SIDE; ny (9.2% of neutral areas, (pavapeni 119-1 at C)). The predicted method eliminates the multiplicity of the process and allows puffing Pinosypvina wfir concentrates with a yield of 20–25% of neutral liquids of 82–93% purity. Repeated chromatography on a syligel with added (3–5% -nr aaorv acid) gives shnosilvine surfactants with 15–22% neutral liquor content 98-99.5% purity .., .ovjj; Formula and 3 o b e te n E tim metilovk vfirov pivosilvyna vkstraktsii by-product of sulphate pulp pro duction organic solvent, separating and washing the resulting extra posdedovatelvdo that alkali and water, and 6tgonki rastvfitel vyde tim tseievoIo atografvrovaniem ostatka chrome product, characterized in that increasing the target product ..yu vpsoda and ynpomeHB5rTie "fi6nofH4a: Kbro of the process as a by-product of the sulphate pulpis - production uses black sulfate liquor, and the residue is checked, HenocpejicTBeiaBc tto cne is removed from the solvent. . - - -: c .-; .. ---., -, .- Sources; information taken into account in the examination of A. I. Lisin et al. Extractive Wood Substances, Lime, Siberian Branch of the Academy of Sciences of the USSR, 1970, No. 12. p. 121-122, 2. USSR Author's Certificate No. 425893, cl. C O7 C 43/20, 1972 3 L. n. Conner, a.W .. ,, QiC NeutPats in Sowthei Taty, 3. of the Ltert. OVe Chem.Soc. , 1975, No. 9, p, 334-337.