SU713870A1 - Method of preparing bis-(benzeneosmium dichloride) - Google Patents

Description

(54) METHOD FOR OBTAINING BIS (BENZENEACOBIDIDE CHLORIDE)

The invention relates to a new process for the preparation of bis (benzolithium dichloride), which can be used as a catalyst for the hydrogenation of unsaturated compounds. The known method is better than bis (benol osmium dichloride) by the interaction of osmium trichloride with cyclohexadiene--1.3 in alcohol at 8 ° C for 5-6 h. The yield of the desired product is 5% l. The disadvantage of this method is the low yield of the target product. The technical essence and the achieved result of the proposed method is the closest to the method of obtaining bko. (benzolium dichloride), which involves the interaction of the trichloride osmium polyhydrate with cyclohexadiene-1,3 in contact at 45 ° C for 5-6 h. The yield of the desired product is 68% L.2. The disadvantage of this method is the use of hard-to-reach unstable polychloride trichloride osmium which is obtained with poor output by heating the osmium tetroxide with con- centered hydrochloric acid at 12 Cp for 48 hours. In this case, Olsb.- is formed as a by-product that is difficult to clean and isolate in the crystalline form. de. In addition, the osmium tetroxide used is a very toxic and highly volatile substance. The aim of the invention is to simplify the process. Goal achieved; the method of producing bis (benzolimide dichloride), which consists in the fact that sodium hexachlorophosphate, tin dichloride in a 1: 1 ratio, is treated with cyclohexadiene-1.3 in an alcohol medium at 4 ° -80 ° C. The yield of the target product is 65%. PRI me R. A solution of 2.25 g (5 mmol) of sodium hexachlorosmate and 0.9 5 g (5 mmol) of dichloride in 100 ml of alcohol is placed in a flask equipped with a stirrer. To the resulting mixture was added 5 ml of hadcohexadiene-1,3 and stirring

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VJT at 40-80C for 5 hours. The mixture is then filtered, the filtrate is evaporated in vacuo, the residue is crystallized with aletonitrile-ether. Obtain 0.97 g (65% of theory, counted as reacted sodium hexachlorosmate) bisSbenzblosium dichloride), t. 210-220 ° C. The IR spectrum (KBf) contains bands

: npH 3055, 2970, 2915, 1430, 1134, 104O, 1005.86O, 6 50 cm. NMR specter

; ): singlet pr-; b 5.35 m „d. literary data; tf 206-209 С IR spectrum: ЗО55, 2970, 2915, 143О,

: 1134, 1O40, 1OO5, 860, 650 NMR spectrum (CH „СЫ): singlet at (5 5.35 ppm)

Found%: C 2O, 85 | H 1,8O.

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All-Isleno,%: C, 21.25; H 1.78. The use of the proposed method for the production of bis (benzopromium chloride) provides, in comparison with known methods, the simplification of the process due to the production of sodium hexachlorosmate produced in industry, with the exception of

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a process of unstable, hard-to-reach polyhydrochloride trichloride (osmium, for the synthesis of which very toxic osmium tetroxide is used.

Claims (2)

Invention Formula The method of obtaining bis (benzolimidi-10 chloride) from 1 cyclohexadiene 1, 3 with the compound osmi in an alcohol medium when heated, so that, in order to simplify the process, as a compound os-ts mi use sodium hexachlorosmate in SMESK with bilayer tin at WITH in relation to Itl, the process is carried out at a temperature of 4 0-8 O C, Sources of information, 20 taken in attention during examination l.Z.NaturiorscVi, 2iiliiO9 (1966). 2. Rubles A. 3 and others. QuiTea al nlbenzolosimiykhloridov, ed. Academy of Sciences of the USSR, 25 ser. chemical .. 1974, 1902 (prototype;