SU598897A1 - 4-(n-carboxyphenylsulfone)-naphthalic anhydride as semiproduct at synthesis of heat-resistant nitrogen-containing heterogeneous ring polymers and method of obtaining same - Google Patents

Description

..- .. .. . (v Litsilirovany acenaphthene with toluensulfonyl chloride is carried out according to the reaction of the Craftsman in the presence of a catalyst by heating equimolar amounts of Iyenaften and toluene ulfluhlidea with gradual heating to. To increase the yield of the target product, the reactionHydromate in the presence of anhydrous synthesis in the presence of anhydrous acid. The background is carried out with potassium permanganate in pyridine, usually with the addition of small amounts of a 1% strength solution of KOH. The use of pyridine makes it possible to obtain an oxidation product with a high yield (72%). The obtained 4- (p-carboxyphenylsulyl background) naphthalic anhydride is dried and "eued" with lOO-iSO C to the foam of the oxidation product in an aqueous alkaline solution. The structure of the compound obtained is confirmed by elemental analysis, titration, IC-spectroscopy data. Preparation of 4- (p-carboxyphenylsulfone) naphtadeo5B1O o, anhydride. A mixture of 6.2 g (0.04 mol) of ace aften "7.0 g (0.04 mol). Toluenesulfonyl chloride and 16 g of anhydrous Cr-Sbd are slowly heated. before . Upon termination of the release of eodoride chloride, the contents of the flask were cooled / cooled to room temperature and treated with a 30% solution. The OH- solid was separated by filtration, washed with water and dried. After repeated recrystallization from toluene, tpl “Yield 80% of the theoretical. Calculated,% "C 74,0; H 5.2, C, HL.O S Found,%: 73.5 H 5.0.

3000.56 410

3500, / tf

430

500 0.31-0.37 450

Solubility

D1MF DMA

H, SO

nsoon

HP HP

Р Р

pH HP HP

HP HP

RI A three-neck flask equipped with a stirrer, a thermometer, a reflux condenser, and a separatory funnel was added 3.08 g (0.01 mole) of 5-acenaphto or p-tolylsulfone and 70 ml of pyridine. The contents of the flask are mixed until complete dissolution at. For 30 g. 1in add 2.0 g (10, at the same time drop by drop 50 ml of 10% solution. KOH. The reaction is stirred at 70-75 ° C for 2-W, then 100 -150 mp of water, distilled, aqueous pyridine and WhOa filtered. The filtrate was acidified with concentrated H to pH 6-7. The precipitate was filtered off and dried at SO-C. 72% yield of theoretical. The resulting product was dissolved in a 5-nanometer KOH solution. , boiled with activated charcoal and 4- (p carboxylphenylsulfone) naphthalic anhydride is separated from the solution with HSE after several times dependencies of KOH, mp 214-21, calculated O% C 59.68; H 2, b4g S8.39 SAoO, S Found,% g C 59.41; H 2.50; 38.43. Acid number 4- {p-carboxyphenylsulfone) naphthalic anhydride 436.0 (theory. 440.6). test of 4- (p-carboxyphenylsulfone) naphthalic anhydride as an intermediate for the synthesis of heat-resistant nitrogen containing heterocyclic polymers. The indicated compound is used as an intermediate for the synthesis of heat-resistant polymers. 3f 3, 4 4 4 tetrasparate rd1 rd is used as nucleophilic polycondensation in the synthesis of polymers. and 3 f 3-diaminobenzidine (DAV) -. Polycondensation is carried out. in a PFC solution at 180–200 c during the structure of the polymers obtained, the data of elemental analysis and IR spectroscopy are confirmed. In Table. 1 shows the main characteristics: terist1-1ki of the polybenzimidazolonaftoklenbenzimidaeloz (PNNI) obtained in comparison with limestone. Table 1

High molecular weight, good solubility and relatively low softening temperature while maintaining high heat resistance contribute to the widespread use of the polymers obtained in the production of film and compression materials.

The use of PNBI obtained on the basis of DAA and 4- (p-carboxyphenylsulfone) naphthalic anhydride has a positive effect on such important technical characteristics as the specific impact viscosity and tensile strength during static bending.

Comparative characteristics of compression materials are given in Table. 2

T a b l and c a

Claims (2)

Invention Formula 1. 4- (p-CarbOxyphenylsulfone) naphtha left anhydride of the formula noos as an intermediate in the synthesis of heat-resistant nitrogen-containing heterocyclic polymers. 2. The method of preparing the compound according to Claim 1, that is, that acenaphten is treated with toluene sulfochloride with a gradual increase in temperature from room temperature to tin in the presence of 4-tin chloride, the resulting product is oxidized at bz-tbc potassium permanganate in pyridine solution followed by boiling the oxidation product with an aqueous alkaline solution. Sources of information taken into account during the examination 1 USSR author's certificate 300487, cl. C 08 Q 20/32, 30 ..