The method of producing tetraphenylporphine indium (iii) acetate

 

(57) Abstract:

The invention relates to methods for future products, for example, as sensitizers for organic semiconductors. Synthesis of tetraphenylporphine India (III) of lead acetate in glacial acetic acid at the boiling temperature and the stirring of equimolar quantities of tetraphenylporphine and nanopowder India obtained by electrical explosion of wire in an inert gas. The technical result - simplifying the process and increasing the yield of the main product. table 1.

The invention relates to a method of producing tetraphenylporphine indium (III) acetate (Cfpps3COO -), an analogue of which chlorophthalazine chloride known as the sensitizer organic semiconductors [Appl. phys. hell 46 (2), January 1985, p. 196-197, M. Kato, Y. Nishioka, K. Kaifu, K. Kawamura, S. Ohno].

There is a method by which octaethylporphyrin indium (III) hydroxide (Oeppen) obtained from octaethylporphyrin (EIA) indium (III) chloride in the medium of dimethylformamide (DMF) when heated to 180-190oC for 4-6 hours. The outlet 80% [J. H. Fuhrhop and K. M. Smith.- In: Porphyrins and metalloporphyrins./ Ed. K. M. Smith Amsterdam etc.: Elsever, 1975, p. 797].

The disadvantages of this method is the high temperature, duration% (III) chloride (InCl) from tetraphenylporphine (DFT) and InCl3in the phenol for 2 hours [Lomov I.e., Berezin B. D. advances in the chemistry of complex compounds of porphyrins with multiply charged cations p-, d - and f-metals. Coordination chemistry, 1993, T. 19, N3, page 173].

According to this method, along with the main product in large quantities ( 50%) is formed admixture of tetraphenylboron indium (III) chloride (InCl), which makes it difficult to erase the primary product.

The task of the invention is to develop a method of producing tetraphenylporphine indium (III) acetate (Cfpps3COO), allowing to reduce the temperature, reduce reaction time and increase the yield of the main product.

The technical result is achieved by the fact that the synthesis Thmpsn3COO lead in glacial acetic acid at t = 118oC for 10 min in the interaction equimolar quantities nanopowder (NP) India obtained by electrical explosion in the atmosphere of nitrogen or argon, with DFT, and NP India pre-dispersed with an ultrasonic disperser in the environment of glacial acetic acid for 1 minute.

Way of the following examples.

Example 1. To 0.12 g (0.001 mol) nanopowder India with Sbeats= 4.5 m2g, obtained by the method of electric is by using an ultrasonic disperser, within 1 minutes Heated to t = 118oC with constant stirring, add 0.3 g (of 0.0005 mol) DFT. The synthesis of the lead 10 minutes before the disappearance of the absorption bands DFT in the electronic absorption spectrum of the reaction mixture.

The reaction mixture is cooled to room temperature, the resulting product is extracted with chloroform. Purification of the reaction product is carried chromatographytandem solutions of the complexes on Al2O3, dried at 50oC. the product Yield of 95%.

Example 2. To 0.12 g (0.001 mol) nanopowder India with Sbeats= 2.0 m2g obtained by electrical explosion of a conductor in an argon atmosphere, add 20 ml of glacial acetic acid. The mixture is stirred using an ultrasonic disperser for 1 min Heated to t = 119oC with constant stirring, add 0.3 g (of 0.0005 mol) DFT. The synthesis of the lead 10 minutes before the disappearance of the absorption bands DFT in the electronic absorption spectrum of the reaction mixture.

The reaction mixture is cooled to room temperature, the resulting product is extracted with chloroform. Purification of the complexes is carried chromatographytandem solutions of the complexes on Al2O3, dried at 50oC. the product Yield of 95%.

The position of the bands with the electronic absorption spectrum policy InCl [Lomov I.e., Berezin B. D. advances in the chemistry of complex compounds of porphyrins with multiply charged cations p-, d - and f-metals. Coordination chemistry, 1993, T. 19, N 3, S. 178].

The spectrum obtained Thmpsn3COO identical in the number and position of the vibration frequencies literature data for tetraphenylporphine metals [G. N. Gurinovich, A. N. Shevchenko, K. N. Soloviev. Spectroscopy of chlorophyll and related compounds, Minsk, 1968, pp. 80-113].

The proposed method allows to reduce the reaction time is 10-12 times and to increase the yield of the final product.

The method of producing tetraphenylporphine indium (III) acetate, wherein the nanopowder India obtained by electrical explosion of wire in an inert gas dispersed in glacial acetic acid, the mixture is heated to the boiling temperature of acetic acid and subjected to interaction with equimolar number of tetraphenylporphine under stirring.

 

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