SU295764A1 - A METHOD FOR OBTAINING SILICON CONTAINING GL AND KOL CARBAMAT AND ALL-UNION: HUH ^ E1 hl-rt. - Google Patents

Description

The invention relates to the synthesis of new carboxy-functional nitrogen-containing silicon compounds, in which a mixture of oxyethyl and carbamathium groups of general formula R 3 Si (CH 3) 2 NHCOOC 2 H 40 H, where R is alkyl, is alkoxy.

The synthesis of niochium silicon / 1 AlCl and Si-derivatives of carbamic acid is known by hydrosilylation of N-allyl or 0-allylurethanes or amylation of organic crepium chloroformates.

Odiac silicon-containing glycol carbamates were not previously produced. They can be used as a cremium / scavenger monomer, which cannot be used to modify the properties of known i-polymer materials (iolamides, iol esters, nolysiloxanes), and also as starting materials for obtaining polysiloxanes with glycolcarbamate groups.

The proposed removal method consists in that the silicon orylamine amines are reacted with ethyl acarbonate to isolate the target product by known methods. It is better to carry out the process and heat up to 60-80 ° C. It is regulated1; it is possible to direct the temperature process and the process towards the formation of either monomers or

oligomeric siloxanes with glycolcarbamate groups.

Example 1. y-triethylsilylnroiylcarbamic acid p-hydroxyethyl ester

(I).

A mixture of 8.7 g of triethylsilylpropylamine and 2.9 g of zinc lencarboiata is extracted for 6-8 hours at. Fractionation yields 6.2 g (82%) of compound I with m.p. 174-175 ° C at a pressure of 1 mm RT. Art., Pr ° 1.4720, d4 ° 0.9937; iMRD 73.67, calculated MRn 74.34. Found, “/ c: N 5.48.

CiaHarOsNSi. Calculated,%: N 5.35.

PC spectrum (slg-1): 734, 1246 (Si-C); 1720, 1540 (I, P amide bands C O; wide with hair center with 3343 (OH and NH).

Example 2. (3-Hydroxyethyl ester of y-methyldiethylsilylpropylcarbamic acid (P).

Under similar conditions, 7.5 g (78 ° / o) of Compound II with 6.4 g of diethylmethylsilylpropylamcium and 1.8 g of ethylene carbonate are obtained.

20

m.p. Irie pressure 1 li1 rt. Art., n 1 ,, df 0,9992; MRo 68.93, calculated MR

69.67.

IR (cM-i): 751, 802, 1245 (Si-C); 1710, 1547 (I, II amnd bands of C 0); wide strip with center 3350 (OH and NH).

Example 3. Y-triethoxylylylpropylcarbamic acid (III) pTydroxyethyl ester.

An equimolecular mixture of 3 minopropyltriethoxysilane and ethylene carbopate is kept for 3-5 hours at 40-50 ° C in an inert gas atmosphere. The crude compound III is obtained.

Found,%: C 44.88; And 8.84; Si 10.29. C, 2ll2706NSi

Calculated,%: C 46.57; H 8.79; Si 9.07.

IR spectrum (gf): 1255 (Si - C); a set of frequencies in the region of 1085-1140 (Si-O, C-O); 1712, 1540, (I, II amide bands With O); wide strip with center 3335 (OH, NH).

Example 4. Synthesis of oligosiloxanes on the basis of y-triethoxylylpropylcarbamic acid | 3-hydroxyethyl ester.

p-Hydroxyethyl ester of Y-triethoxysilylpropylcarbamic acid is heated (150-160 ° C) under vacuum (1-2 mm of mercury) to

excretion of a certain amount of ethanol. A mixture of oligosiloxanes is obtained in the form of a thick viscous liquid.

o / o: C 34.83; H 6.25; Si 15.19;

Found, N 6.26.

CeHisOsNSi: C 34.94; H

5.86; Si 13.61;

Calculated N 6,79.

IR spectrum (s): 1255 (Si-C); wide band in the region of 1140-1045 (Si -O, C -O); 1710; 1545, (I, P amide bands); wide strip with center 3345 (OH and NH).

Subject invention

Claims (2)

1. A method for preparing silicon-containing glycol carbamates, characterized in that Y-aminopropylsilane is reacted with ethylene carbonate, followed by isolation of the target product by known methods. 2. A method according to claim 1, characterized in that the process is carried out by heating, for example, to 60-80 ° C.