SU427014A1 - METHOD OF OBTAINING HETEROCYCLIC TRISULPHONES - Google Patents

Description

one

The invention relates to a method for the production of heterocyclic trisulfones not contained in literature, which can be used as intermediates in organic synthesis.

There is a known method of obtaining substituted trisulfonylmethanes, which consists in the fact that the corresponding Mercaptan is condensed from derivatives of formic acid in the presence of anhydrous HC1, followed by oxidation of the obtained tritiorortoformate with an excess of peracetic acid in ecu medium at (-20) - (- 30) ° C and isolation of the target product in a known manner.

A method is proposed for preparing heterocyclic trisulfones, in that the oxydimethylenediamine sulfate is condensed with the appropriate n-octyl alkyl sulfide ketone under cooling in the presence of ethanol containing 15% hydrogen chloride, with the following oxidation obtained from x-methyl methyl sulfide-4 -methyle-4-methyl-chloride, obtained using xyloxymethyl-4 -methylene-methyl chloride, obtained using the following oxidation obtained from x-methyl methyl sulfide-4 -methlymethyle-4-methyl chloride, obtained using the following oxidation of the resulting xydine methyl omethyl-methyl chloride, obtained using xyloxymethylene-methyl chloride, obtained using xanthine methyl sulfide -methly -methlymethylomethylomethyl chloride, with the following oxidation of the resulting xydine methyl omethylmethylomethylammethylomethylomethylochloride, obtained the following oxidation using hydrogen in glacial acetic acid and release of the target product in a known manner.

The condensation process should be carried out at a temperature of (-5) - (-7) ° C.

When Mer. Sodium methyl oxydithiosulfate and the corresponding n-octyl alkyl sulfide ketone are introduced into the cholba, followed by

external cooling to -5 ° C and private stirring to the reaction mixture is applied; 100 g of ethanol containing 15% HC1 is used. The reaction ends after 4 hours. After the reaction has been quantified, the contents of the flask are left for 6 hours at commatized temperature, then transferred to a 1 L flask, filled with water and left for 6-8 hours at room temperature. The precipitate obtained is filtered on a Buchner funnel, washed with cold water and dried. The dried product is extracted with hot benzene in a Socket device.

After extraction, adduct 1 is isolated; 1 addition of 1 mol of sodium oxpmethylenedithiosulfate to n-octyl alkyl sulfide ketoi, represented by white heavy needle shiny crystals with a specific odor. Upon subsequent oxidation of the adduct with hydrogen peroxide in ice and acetic acid, the corresponding trisulfones are obtained in the form of white polycrystals with an insignificant specific odor.

As an example, IR spectra of pequot are taken ;; In this case, nolos are intense in the spectrum of nolos for 1140, 1181, 1212 s. characterizing the SOo group.

Properties of the compounds are shown in the table. The subject matter of the invention is 1. A method for producing heterocyclic trisulfones, wherein the oxidimethylenedithiosulfate is condensed with the corresponding n-octylalkylsulfide ketone under cooling in the presence of ethanol containing 15% hydrogen chloride, followed by oxidation of the half-hydroxymethylene disulfide methyl isomethyleneglymethyl sulfate. acid 1 by isolating the desired product in a known manner; 2. Method no. 1, characterized in that the condensation process is carried out at a temperature of from -5 to -7 ° C.