SU643508A1 - Method of obtaining 1-acyloxystannantanes - Google Patents

Description

one

The invention relates to a floor method; new compounds, namely 1 acyloxistannanes of the general formula

RCOOSn (OCH, CH5), N

(I).

t 23,

where R is lower alkyl, which can be used as biologically active substances and components of catalytic systems.

The known method flj for the preparation of 1-hydrosilatran by the interaction of trialkoxy silanes with 2, 2, 2-aminotrialkoxyboranes of the general formula

.CH (R) 03jB (I). Ii

The disadvantages of the method are the limited scope, duration of the process / and also the need to carry out the process at temperatures above 100 ° C in the presence of a catalyst.

The purpose of the invention is to create a method for producing new type compounds with valuable properties.

This is achieved by the fact that in the process for the preparation of compounds of general Formula

RCOOSntOCHjCH,), P,

t1.

where R is lower alkyl, tin tetraacylate of the general formula

SnCOOCR) (f),

where is lower alkyl, is reacted with tris- (2-trialkylstanoxyethyl) amine of the general formula

NtCH CHjOSnRjIj

where R is lower alkyl, in an inert organic solvent environment in an inert gas atmosphere.

. The yield of the target product is 85-92%. The desired product is isolated by known techniques. The resulting trialkyltin acyllate as a by-product of the general formula

(V)

R, StiOOC

where R is lower alkyl, is again converted to the starting Tris- (2-trialkylstanoxyethyl) amine of the general formula (IV)

The previous method allows the reaction to be carried out in aprotic organic solvents at room temperature and in the absence of catalysts using readily available tetraacylates of tin and tris (2-trialkyl stanoxyethyl) amine as starting materials. The latter is regenerated from the mixture in a yield of about 80%.

The proposed method allows to obtain, with a high yield of easily available starting materials, a new type of compounds that are of interest in various technical fields.

1 Acyloxystannatranes can be used as biologically active substances, components of catalytic systems, lubricant additives, initial products in the synthesis of various tin derivatives.

Example 1. Synthesis and purification of the substance is carried out in an atmosphere of dry iredtnogo gas. To a solution of 6.16 g (0.015 mol) of tin tetrapropionate in 5F ml of benzene with dripping was added dropwise 15.233 g (0.015 mol of tris- (2- tri-n-butylstanoxyethyl) amine in 80 ml of ether. The separated precipitate is filtered off, washed with serum and dried in vacuum. The yield is propionate 85%, melting (with decomposition, in a sealed potassium).

Found,%: C 32.07; H 5.01; N 4.26; Sh 35.25.

CoN "MO 5P.

C, 31.98; H 5.03; N

Calculated% 4.15; Sn 35, 16..

The substance dissolves well in cold in methanol, ethanol, acetic acid, chloroform and pyridine, and when heated in dioxane; in water, acetone, ether, carbon tetrachloride, aromatic hydrocarbons, tetrahydrofuran, hexane, and petroleum ether, it is poorly soluble even when heated.

From the filtrate, 11 g (82%) of hexa-n-butyldithAHHOKcaHa, dissolved in 100 ml of toluene, were added by conventional methods, 1.84 g of triethanolamine was added, the mixture was boiled for 40 minutes, the water and toluene formed were distilled off in vacuum to constant weight. 12.47 g (81.8% of the starting material prepared for the reaction) Tris- (2-tri-n-butylstanoxyethyl) are obtained. amine in the form of an oily liquid light yellow color with

and 1.4943.

Found,%: C 49.81; H 9.14; M 1.52; Sn 35.28.

С, Н „

Calculated,%: C 49.65; H 9.16; N 1.38; Sn 35.07.

Example 2. 1-Isobutyratestannatran was prepared analogously to 1-propionate-natanate from 12.6 g (0.027 mol) of tin tetraisobutyrate in 150 ml of ether and 27.4 g (0.027 mol) of tris- (2-trine butylstanoxy ethyl) amine. Yield 8.81 g (92.7%), m.p. 204 ° С (with decomposition in the injected capillary).

Found,%: C 34.06; H 5.49; N 3.87; Sn 33.66.

,, NO SnCalculated,%: C 34.11; H 5.40; N

3.97; Sn 33.74.

From the filtrate, 23.02 g (84 Tris- (2-tri-n-butylstanoxyethyl) amine) were obtained, with g 1.4946.

Claims (1)

1. USSR author's certificate No. 192209, cl. C 07 F 7/22, 1967.