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United States Patent (19) 11 Patent Number: 4,755,589 Sandman (45) Date of Patent: Jul

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United States Patent (19) 11 Patent Number: 4,755,589 Sandman (45) Date of Patent: Jul United States Patent (19) 11 Patent Number: 4,755,589 Sandman (45) Date of Patent: Jul. 5, 1988 (54) AROMATIC SELENUM COMPOUND POLYMER OTHER PUBLICATIONS Balodia et al., J. Org. Chem. USSR (Engl. Transl.) 15, 75 Inventor: Daniel J. Sandman, Acton, Mass. 343 (1979). Gladysz et al., J. Org. Chem. 43, 1204 (1978). Assignee: GTE Laboratories Incorporated, Battistoni, P. et al., Gazz. Chim, Ital. III, 505 (1981). 73 Sandman, D. J. et al. (1982) J. Chen. Soc., Chem. Com Waltham, Mass. mun. pp. 1133-1134. Ohnishi, S. et al. (1982) Chemistry Letters, pp. (21) Appl. No.: 870,122 1841-1842. Endres, H. et al. (1982) Mol. Cryst. Liq. Cryst. 86 22 Filed: Jun. 3, 1986 111-122. K. Y. Jen et al., J. Polymer Sci., Polymer Lett. 21, 441 (1983). Related U.S. Application Data S. Tanaka, et al., Makromol. Chem., Rapid Commun. 4, 62 Division of Ser. No. 507,156, Jun. 23, 1983, Pat. No. 231-235 (1983). 4,597,914. T. Hasegawa et al., J. Polymer Sci., Polymer Lett. 22, 365 (1984). (51) Int. Cl* .............................................. CO8G 83/00 Primary Examiner-Harold D. Anderson 52) U.S. C. ................. ... 528/397; 528/388 Attorney, Agent, or Firm-Hamilton, Brook, Smith & 58 Field of Search ...................... 528/397,388 Reynolds 56) References Cited 57 ABSTRACT U.S. PATENT DOCUMENTS This invention constitutes a method for preparing mo lecular and polymeric aromatic selenide compounds 3,149,101 9/1964 Hubel et al. ........................ 260/239 such as bis-phenyl selenide and poly(p-phenylene sele 3,354,129 11/1967 Edmonds et al. ................... 528/265 3,790,536 2/1974 Vidaurri.............................. 528/388 nide). The method comprises reacting an aryl halide 3,965,049 6/1976 Grushkin et al. ....................... 520/1 with an alkali metal selenide reagent formed in an 4,344,869 8/1982 Binne et al. ........................ 252/517 aprotic solvent. 4,540,620 9/1985 Johnson et al. ..................... 528/388 4,597,914 7/1986 Sandman ............................. 528/397 2 Claims, No Drawings 4,755,589 1. 2 synthesis of these compounds under significantly milder AROMATIC SELENIUM COMPOUND POLYMER conditions. This application is a division, of application Ser. No. BEST MODE OF CARRYING OUT THE 507,156 filed June 23, 1983 now U.S. Pat. No. 4,549,914. 5 INVENTION The alkali metal selenide reagent is formed in an DESCRIPTION aprotic solvent such as N,N-dimethylformamide, hex 1. Field of the Invention amethylphosphoramide or N-methylpyrrolidinone. This invention is in the field of organic chemistry and Finely divided elemental selenium is added to the sol relates to methods of synthesizing organometallic com 10 vent, and a suspension of selenium is formed by stirring. pounds containing selenium. Specifically, it relates to a The suspension is heated to about 100 C. and then method of synthesizing molecular and polymeric aro pieces of alkali metal are added to form a mixture in matic selenium compounds and a reagent useful in the which the molar ratio of alkali metal to selenium is preparation of such compounds. about 2:1. The resulting alkali metal selenide has the 2. Background of the Invention 15 chemical formula M2Se wherein M is an alkali metal. Poly(p-phenylene sulfide)(PPS) is a crystalline, aro The alkali metal employed in the production of the matic polymer comprising benzene rings linked with intermediate selenide reagent may be lithium, sodium or sulfur atoms in the para position. The polymer exhibits potassium. Sodium however is the preferred metal be several advantageous properties including high-temper cause it is most convenient to use. ature stability, flame resistance and good chemical resis 20 The reaction to form the alkal metal selenide reagent, tance. PPS is used widely as a coating material and in and the reaction of the alkali metal selenide reagent injection and compression molding processes. Recently with the aromatic halogen compound may be carried PPS has received attention as an example of a polymer out in the same solvent. Thus, after the reagent is syn without a continuous carbon ar system which becomes thesized, the aromatic halogen reactant is added di highly conducting on exposure to strong oxidants. See 25 rectly to the reaction mixture containing the alkali e.g., European patent application No. 80107176.2. metal selenide reagent. The entire synthetic procedure The usefulness of PPS has generated interest in the may be carried out under an atmosphere of an inert gas selenium analog of PPS, poly(p-phenylene selenide) such as argon or one of the other noble gases. This (PPSe). At least one unsuccessful attempt to prepare prevents undesirable side reactions with moisture or the PPSe from Na2Se and p-dibromobenzene in ethyl ace 30 components of air. tate solution has been reported See, Okamoto et al., After the intermediate alkali metal selenide reagent is Ann. N.Y. Acad. Sci 192:60 (1972). Balotis et al. have reacted with an aromatic halogen compound to form reported the synthesis of the metallocyclic compound the desired molecular or polymeric organic selenide, tetraselenotetracene from sodium diselenide (Na2Se2) in the product is then separated from the reaction mixture dimethylformamide solution. 35 by conventional techniques. For the most part the re sulting selenide compounds are not air-sensitive and SUMMARY OF THE INVENTION therefore may be subjected to purification techniques This invention constitutes a method for the synthesis such as recrystallization, sublimation or the like without of conjugated molecular and polymeric aromatic sele 40 exercise of excessive care. nium compounds. The method involves the reaction of According to the method of this invention, bis aryl aromatic halides with an alkali metal monoselenide selenide compounds are produced by the alkali metal reagent such as Na2Se or K2Se. According to the selenide reagent with a monohaloaromatic compound. method of this invention, the alkali metal selenide rea The reaction between the alkali metal selenide and the gent is formed directly from an alkali metal and sele 45 aryl halide in a molar ratio of substantially 1:2 gives nium in a polar aprotic solvent, and the reagent is then products of the general formula Ar-Se-Ar where Ar reacted with an appropriate aromatic halide in the same signifies the particular aromatic group of the aryl halide solvent system to form the desired molecular or poly reactant. The synthesis of bis aryl selenides is typified meric organic selenium compound. by the reaction of 2-bromonaphthalene with sodium Examples of some of the molecular aromatic sele 50 selenide to give bis-(3-naphthyl)selenide. nides which may be synthesized by this method are bis-phenyl selenide, bis(2-naphthyl) selenide and bis(9- anthracenyl) selenide. Molecular aromatic selenides Br have useful bactericidal activity, antiseptic activity and anti-inflammatory activity. See e.g. "Organic Selenium 55 Compounds: Their Chemistry and Biology" ed. D. L. Klayman and W. H. H. Gunther, Wiley-Interscience Se (1973). Examples of some of the polymeric aromatic selenides which may be produced are poly(p-phenylene -- 2NaBr selenide) and poly(9,10-anthraceneselenide). Polymeric aromatic selenides are precursors to conducting poly e.S. Aromatic polymers are produced by reacting the The invention provides a simple and direct method alkali metal selenide. reagent with a dihaloaromatic for synthesizing previously-known and new or compound. The reaction between the alkali metal sele ganoselenium compounds. The method eliminates the 65 nide and the dihalo-aromatic compound in a molar ratio use of liquid ammonia or other nitrogenous solvents, of substantially 1:1 gives polymeric aromatic selenides which are used currently in the synthesis of or of the general formula Ar-Se-n. The synthesis of ganoselenium compounds, and thus provides for the organic polymeric selenides is typified by the reaction 4,755,589 3 4. of p-dibromobenzene with sodium selenide to give Calculated for -C6H4Se-n: 46.48; H, 2.60; Se, 50.92. poly-(p-phenylene selenide) (PPSe) Observed: C, 41.36; H, 2.26; Se, 52.15; Br, 1.57. The observed elemental analysis corresponds to a Br composition of C60H3.91Sel. 15 and based on bromine 5 analysis, a molecular weight of 5000 or 10,000 is esti mated for one and two bromine atoms per polymer chain, respectively. The 15% atomic excess of selenium + Na2Se-G- -KO)-- is attributed to diselenide linkages in the polymer. The x-ray diffraction pattern of this polymer is similar to Br O that described in Example 1 and shows no elemental As shown in the equation, p-dibromobenzene reacts selenium. with the sodium selenide reagent to form PPSe. Nota EXAMPLE 3 bly, these reaction conditions are significantly milder Preparation of PPSe from p-dichlorobenzene in than those used for the synthesis of poly(p-phenylene 15 sulfide) (PPS). It is suspected that the facility of the N,N-dimethylformamide (DMF) reaction is due to the operation of an SRN1 mechanism. A sodium selenide reagent was prepared in DMF (40 The polymeric selenides, such as PPSe and poly(9,10 ml) in the usual manner from selenium (2.17 g, 0.0275 anthraceneselenide), are useful as precursors to con gm-atom) and sodium (1.30 g, 0.055 gm-atom under ducting polymers. For example, exposure of PPSe to 2O argon. To this reagent was added p-dichlorobenzene arsenic pentafluoride (at 100 Torr) for 5 hours at 40 C. (3.675 g, 25 mmole) This mixture was kept at a bath results in a conductivy for the treated polymer of about temperature of 140-145 for 18 hours and then at 10-2-10-3 (ohm cm)- 1. B 170°-175 for 100 hours. The product was isolated as The following specific examples further illustrate the previously described to give PPSe as a light brown invention.
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