SU415272A1 - METHOD FOR OBTAINING ALLYL CARBONILGALOID COMPLEXES OF PALLADIUM - Google Patents

Description

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The invention relates to a process for the preparation of new palladium derivatives, in particular allylcarbonyl halide complexes of the formula

(C3H5) Pd2 (Hal) 2 (CO)

where Hal is halogen, which can be used as a catalyst or donor of the CzNb and CO groups in the synthesis of more complex organic or organometallic compounds.

A method of obtaining allylcarbonyl chloride complexes of palladium in an atmosphere of air of the general formula

(C3H5) Pd2Cl2 (CO) 2.

According to the above formula, in the compound one of the palladium atoms coordinates the allylic grouping CsHs, and the other - two CO groups.

It is also known that Pd (II) coordinates only one CO molecule, and therefore the compound obtained is either a mixture of the original allyl compounds of palladium and palladium carbonyl chlorides formed under these conditions, or the second CO molecule is introduced through the C-Pd bond with the formation of organometallic fragment.

This explains the fact that the authors who obtained the compound (C3H5) Pd2Cl2 (CO) 2 do not indicate the yield of the target product.

In addition, it is known that carbonyl and allylic palladium complexes are very unstable in air.

Describes a method for producing allylcarbonyl halide palladium complexes, concludes that allyl dihalide palladium is treated with carbon monoxide under an inert gas atmosphere in an organic solvent medium to give the desired product.

famous tricks.

The solvent is released from oxygen by purging with nitrogen. Product separation and other operations are also carried out in an inert atmosphere. In this, the intermediate carbonyl compounds of palladium are sufficiently stable and can serve as catalysts for the reaction of the carbo; 1, the alkylation of allyl halides palla.ai. In particular, such an intermediate product of PdCOCl composition was isolated.

When applying the proposed method for the preparation of a, 1-l or carbonyl halide palladium halide complexes, existing laboratory facilities can be used.

Example 1. Getting allyldi- (chloropalladium) -carbonyl.

Suspension 2.2 g PdCb. in 150 ml of SIZON and 1.8 ml of CH3SOCI3 are stirred with a magnetic stirrer in nitrogen at a temperature of 20% for 20 ppm. Then 2.3 g of C3H5PdCl2 2 n are introduced.

low CO current with constant stirring at room temperature for 2 h. The entire initial precipitate dissolves, then a light yellow amorphous product precipitates from the solution, which is filtered, washed with ether and dried under high vacuum. The yield of C3H5Pd2Cl2 (CO) is 2.85 g, corresponding to 62% on C3H5PdCl2 2. The product decomposes without melting at 130 ° C.

Found,%: C 13.53; H 1.39; C1 19.60; O 4.70; Pd 60.30.

CsHsPdsCUCCO).

Calculated,%: C 13.65; H 1.42; C1 19.90; O 4.66; Pd 60.6.

Example 2. Getting allyldi- (bromopalladium) -carbonyl.

A suspension of 1.4 g of PdBr2 in 150 ml of SNZON and 0.4 ml of SPZSOVgz is stirred with a magnetic stirrer under a nitrogen atmosphere for 20 minutes. 1.2 g (C3H5PdBr2) 2 is introduced and a weak CO current is passed in with constant stirring at room temperature for 2 hours. The entire initial precipitate is dissolved, then an amorphous amorphous yellow precipitates from the solution.

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the product is filtered off, washed with ether and dried under high vacuum. The yield of C3H5Pd2Br2 (CO) is 1.4 g, corresponding to 64% on C3H5PdBr2 2. The product decomposes without melting at 110 ° C.

Found,%: C, 11.00, H, 1.18, Br, 34.00; O 3.50; Pd 48.50.

C3H5Pd2Br2 (CO).

Calculated,%: C 10.87; H 1.13; Br 36.30; O 3.40; Pd 48.30.

Subject invention

The method of producing allylcarbonyl halide palladium complexes of the formula

(C3H5) Pd2 (Hal) 2 (CO)

where Hal is halo, id, characterized in that the allyldiglode | id is palladium treated with carbon monoxide, in an inert gas atmosphere in an organic solvent medium and the desired product is isolated by known methods.