SU555113A1 - The method of obtaining ferrocene - Google Patents

Description

The invention relates to the synthesis of organometallic compounds, more precisely to an improved method for the preparation of ferrocenophanes, used as preparations that increase the hemoglobin content in the blood.

At present, only two preparative methods for the preparation of ferrocenophanes containing no functional groups are known. One of them is the method of producing ferrocenophanes by reducing cC -carbonyl-containing ferrocenofan with a mixture of lithium aluminum hydride with anhydrous aluminum chloride in an environment of absolute JQ ether. However, this method cannot be applied in industry: highly flammable lithium aluminum hydride and ether are required for the reaction.

There is also known a method for producing ferrocenophanes, which consists in the fact that a ferrocenophane derivative containing an eC-ketone or cC -oxy group is reduced with a mixture of triethylsilane with trifluoroacetic acid, which is also a solvent 2. The yield of the target product reaches 80-90%. The disadvantage of this method is the use of hard-to-reach triethylsilane, as well as the difficulty of purifying the target product from the siloxanes resulting from the reaction.

The aim of the invention is to simplify the process.

This is achieved by the fact that a ferrocenophane derivative containing a cX / ketone or cC -oxy group is reduced with sodium borohydride in the presence of aluminum chloride in tetrahydrofuran and dimethoxyethane or diglyme.

A distinctive feature of the method is the use of sodium borohydride as the reducing agent in the presence of aluminum chloride and carrying out the reaction in tetrahydrofuran or dimethoxyethane or diglyme, however, dimethoxyethane is more convenient. The order of addition of the reagents is not essential M, but the best results are obtained with this sequence: sodium borohydride is added to a solution of the compound to be recovered in dimethoxyethane and then aluminum chloride is added to the pores in the dimethoxyethane.

The proposed method is simple and convenient. Recovery was carried out at a cohogat temperature for a few seconds. which leads to a randomized product. After decomposing the reagent mass with water, ferrschwiofan is isolated in solid wae; the product does not need to be cleaned

Outputs in the recovery of sodium borp-sridam in the presence of "loristus a, immy reach 10%"

It is known that the effect of borohydride on C-hydroxoproxane-ferroceno-s in isopropyl alcohol leads to the formation of the corresponding carbinols or their derivatives - cyclic heteronuclear ether B 3. It is also known that it is used as a solvent; -: sodium ohydride in the presence of fine aluminum in a series of benzene derivatives, not D (lay down carbon-hydrogen derivatives of phenyl, but leads to carbinols 14.

It turned out that lrk soccTaHOBnei-im-i ke-goyN1LH or ether derivatives): ferroaegofan Ooigidri.aom, atriy in the presence of; - l.oristoghe alyuk; iki l. Addition of apuuminmin chloride leads to gsgmu. THAT restoration does not stop iaeTCs-T at the stage of the formation of g of arbinol; And further, As a result, jiofij eHbi - isto hydrocarbon feproce-. aofan;

EXAMPLE: To a suspension of 0.7 - 3-fencl 5-ferrocene fadion - 5 in -40 ml of uH / vis-T9KCH3Ta ia, add 1.4 g of sodium borohydride and then send in small portions with stirring g of Ilyum chloride. After IJ mic, 50 ml of dode 1 50 jvffl diluted oo / th acid is added to the solution. The precipitated -3 fencl SJ ferrocene filter is filtered off and eaten, 0, g of the product (100% of the theoretical) is obtained, Influences on identification of ICTs ano no., Ct, MeToaoivi TLC on ci; .rry4ioae and on .х-: Г MR-spec7 10c spii.

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