SU483409A1 - Method for producing polyphenylquinoxalines - Google Patents

Description

(54) METHOD FOR OBTAINING POLYPHENYLINOXALINES

C-R-C-0 II

with s oII

Cgli.

Cghs

where X O; -; CO, - SOg -;

R is an aromatic radical;

The way polyphenylchloriline oxides are used in chloroform is that the mixture of the starting components is heated at the boiling point of the solvent for 24 hours. The disadvantage of this method is that even multi-hour heating of the solution does not result in a highly molecular polymer, its viscosity does not exceed 0.7.

The goal of this approach is to intensify the process and also to reduce the molecular weight of polyphenyl chloride salts in a solution of chlorinated hydrocarbons, such as tetrachloroethane, chloroform, and methylene chloride. This

The goal is achieved by the use of chlorinated hydrocarbons mixed with substances that are inpOTHOHOiB donors as the solvent in the reaction of aromatic aromatic tetraamines with aromatic bicamines (a-di: ketone and mi), the reaction is carried out at room temperature 2 -3 hours As proton donors, substances selected from the group consisting of methanol, ethanol, phenols, benzyl carbon, organic acids are used. The amount of these substances varies from 1 to 20% (mostly 5-10%) of the volume of chlorinated hydrocarbons. Polyphenylquinoxalines obtained in this way do not differ in mechanical and other characteristics from polymers obtained by dissolving, i-cresol, and have a very high molecular weight of molecules (1 -), p „. 1.3-1.7). The advantage of the proposed method consists also in the fact that in these mixtures, for example, with methanol or benzyl alcohol, these solutions are used in a series of cases to use the reaction solution without hydrofluoric precipitation of the polymer. All polymers are obtained with a hollow entry. PR 51 me er. In a 25-ml three-necked flask, equipped with a stirrer with water for argon, 6 ml of chloroform-methanol (10: 1) are placed, sent to 0.9212 g (0.004 mol) of 3,3,4,4-tetraamipodiphenyl ether another 1 ml of the mixture is added, and then, over a period of 20-30 ° C, 1.7380 g (0.004 mol) of 4.4-bns - (fepylglyoxalil) -diphenyl efirir are powdered. The remains of tetraketone wash off 3 solvents. The reaction mixture is stirred for 3 hours at room temperature, and the polymer is precipitated in methanol or reactive mixture with chloroform, films are poured, iinpuB-1.3 (0.5% solution of i-cresol at 25 ° C). Example 2. By the method described in example 1, from 0.9212 g (0.004 mol) 3,3,4,4 tetraamino diphenyl ether and 1.3692 g (0.004 mol) 1,4-bys- (phenylglyoxalyl) -benzene in a mixture of chloroform-metaiol (10: 1) get the polymer, TinpiiB. 1.7 Example 3. According to the method described in example 1, from 0.9212 g (0.004 mol) 3.3.4.4 tetraamino diphenyl ether and 1.3692 g (0.004 mol) 1,4-b "c- (phenylglyoxalyl a) bent ash in a mixture of chloroform-phenol (10: 1) get g ol; 1.; ep with C: ,,.,.,. 1.5. Example 4. According to the method described in example I, from 0.9212 g (0.004 mol) 3,3,4,4 tetraaminodiphenyl and 1.7380 g (0,004 mol) 4,4-b "c- (phenylglyoxalyl) - diphenyl ether in 10 ml of benzyl siirt receive a half-measure with Yairip. 1.4. PRI me R 5. According to the method described in Example 1, FROM 0.9212 g (0.004 mol), 3,3,4,4tstraamino phenyl eflr and 1.3692 g (0.004 mol) I, -1-bis (phenylglyoxalyl) -benzene in a mixture of methylene chloride - methanol (5: 1) get a polymer with t) "p" ". 1.6. Example 6. According to the method described in example 1, from 0.9212 g (0.004 mol) of 3.3,4.4 tetra-1M1 inod. Fe1P of laval efflora and 1.3692 g (0.004 mol) of 1,4-bis- (phenylglyceloyl) - Benzene in chloroform-acetic acid 40: 1 mixture) a polymer is obtained. Object of the invention Vosa, the reaction is carried out in the presence of substances selected from the group containing methanol, ethanol, phenol, benzyl alcohol, organic acid in an amount of from 1 to 20% by volume of carbon chlorinated hydrogen.