SU371238A1 - METHOD OF OBTAINING COORDINATION COMPOUNDS - Google Patents

Description

one

The invention relates to the field of obtaining coordination compounds of alkali derivatives of gallium with organic compounds of elements of the fifth or sixth group, which are applied in electronic technology.

A known method for producing trimethylgallium 1-coordination compounds with organic compounds of the fifth or sixth group consists in reacting trimethyl gallium with an organic compound of the fifth or sixth group, such as with a trimethyl, trimethyl amine or dimethyl sulphide. The starting compounds are reacted in the vapor state at liquid nitrogen temperature (-195 ° C). The desired product is isolated by known techniques.

With this implementation of the method, the complexity of the process, the need to use low temperatures, the impossibility of obtaining a wide class of such compounds is observed, since the starting metal-organic compounds must be volatile and close in vapor pressure. In addition, in a known manner, it is extremely difficult to obtain coordination compounds of high purity, which makes it almost impossible to use them in electrical engineering.

The purpose of the invention is to control the process technology and increase the purity of the target product.

For this, it has been proposed to use the ester of the alkyl derivative of gallium, 1 reject, being a coordination compound, has a lower reactivity.

The preparation of coordinated compounds of alkyl derivatives of gallium with organic compounds of the elements of the fifth or sixth soil consists in the fact that the ether of alkyl derivative of gallium is subjected to interaction with the organic compound of the element of the fifth of the mccToii group, with the release of the target product by known techniques.

The irost method is reliable in operation, does not require special equipment, it is easy to control and the product yield approaches quantitative.

Example I. Tr. And mn. Of N: i g and. P l and and t r and t t and l m our sh k.

In a reaction flask with a volume of 50 cm, filled with an inert gas, 3.66 g (0.02 mol) of three methyl gallium etherate are placed. 3.24 g (0.02 mol) of triethylmex are gradually added thereto. 1.48 g of diethyl ether, resulting from the coordination of trimethylgallium with a triethylmix, was slowly distilled off. Then, from the reaction flask, the obtained coordination mixture is distilled at 45 ° C and the residual

2mmHg Art. The product yield 5.3 g (98%); 1.4935.

Example 2. Trimethylgallitri3t II l and m and n.

In a reaction flask containing 3.66 g (0.22 mol) of trimethylgallium etherate, 2.02 g (0.02 mol) of triethylamine are gradually added. After diethyl ether was removed by fractionation (1.45 g), the trimethylglyltriethylamine coordination compound remained in the flask - 4 g (96%).

Example 3. Trimethylgallium trimethylmysh.

To 3.66 g (0.02 mol) of trimethylgallium ethoxide, 2.4 g (0.02 mol) of trimethyl mouse are gradually added dropwise. After removal of diethyl ether by fractionation (1.45 g) in a flask, a coordination compound, trimethylgallium-trimethylmuch to -4.3 g (96%), is obtained; m.p. 24 ° C. Example 4. Trimethylgallitrie t and lmyshl to.

To 4.62 g (0.02 mol) of triethyl gallium etherate was added 3.24 g (0.02 mol) of triethyl mouse. After removal of the ester, 6.2 g of triethylgallium triethylshim were obtained; m.p.

(2 mmHg); At 1,5008. Exit 97%.

Example 5. D i m et t and l g and l l and and X l 0r and d t r and et m and l m sh sh k.

To 4.19 g (0.02 mol) of dimethylglychloride etherate, 3.24 g (0.02 mol) of triethyl mouse were gradually added. The ether is distilled at atmospheric pressure. Dimethyl gallium chloride triethyl is distilled under vacuum, yield 96%, 1.5150; m.p. 84 ° C (8 mm Hg. Art.).

Example 6. Trimethylgallium diisoamyl ether.

To 7.32 g (0.04 mol) of trimethyl gallium etherate was added 6.32 g (0.004 mol) of diisoamyl ether. After removal of diethyl ether, trimethylgallium diisoamyl ester was obtained in 95% yield.

The examples given are illustrative of the invention and in no way limit it.

Subject invention

The method of obtaining coordination compounds of alkyl derivatives of gallium with organic compounds of the fifth or sixth group by reacting a gallium derivative with an organic compound of the fifth or sixth group and isolating the product with known techniques, characterized in that in order to influence the process technology and increase purity product, as a derivative of gallium take ether ether alkyl derivative of gallium.