SU320498A1 - METHOD OF OBTAINING TETRAFENOXY-p-ANYLOCYCLICPHOSPHASOTRIENE - Google Patents

Description

This invention relates to a process for the preparation of azo compounds, namely, to a new process for the preparation of tetrafenoxidi-1-anyloxycyclophosphazotriene.

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A method of producing hexaaniloxycyclophosphazotriene by reacting hexachlorophosphazotriene with an alkali metal l-nitrophenol in an organic solvent followed by reduction of the resulting product, for example, on Rene nickel, in an autoclave at a temperature of 80-90 ° C.

The preparation of tetraphenoxy-l-anyloxycyclophosphazotriene, like the compound itself, is not described in the literature and is new. The resulting materials can be used in the chemistry of polymers to produce heat-resistant heteroaromatic polymers.

The method for producing tetrafenoxidi - "- anyloxycyclophosphazotriene is that tetrafenoxyl dichlorocyclophosphazotriene is treated with--acetamidophenol alkali metal in an inert organic solvent, for example, pyridine or xylene, with a body in an inert organic solvent, for example, pyridine or xylene, with a body in an inert organic solvent, for example, pyridine or xylene, with a body in an inert organic solvent, for example, pyridine or xylene, with a body in an inert organic solvent, for example, pyridine or xylene, with a body in an inert organic solvent, for example, pyridine or xylene, with a body in an inert, solvent in an inert organic solvent, for example, pyridine or xylene, with a face in a white, white or white metal in an inert organic solvent, for example, pyridine or xylene, with a face in a white, white or black metal. the selection of the target product known techniques.

The first stage is carried out at 80-150 ° C, saponification at 50-80 ° C. Example 1. A mixture of 17.34 g (0.03 mol tetrafenoxydichlorocyclo phosphazotriene, 9.1 g (0.06 mol) d-oxyacetannlide and 3.63 g (0.06 mol) of solid potassium hydroxide in 120 ml of pyridine was stirred in a flask equipped with an open fridge at boiling of the solvent for 6 hours. The cooled solution after separation of the potassium chloride was evaporated in vacuo (20-30 mm, rt dry). The residue was a very viscous liquid of light brown color, which solidified on cooling to a gummy mass. The crystallized product very slowly crystallized on standing. Crystallization can be significantly accelerated by producing a small amount of acetone or a mixture of acetone and heptane. In the latter case, tetrafenoxydich (ha-acetanyloxy) - cyclophosphazotriene is released as colorless prismatic crystals. Both crystalline and gummy product was identified with

phenoxy- (rt-acetanyloxy) - cyclophosphazotriene. T. pl. crystalline product 160-162 ° C, yield 85-92% (from theory).

Found,%: C 59.15; 59.05; H 4.58; 4.46; N 8.05; 8.40.

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Calculated,%; C, 59.48; H 4.49; N 8.67.

The resinous tetraphenoxy- (p-acetanyloxy) -cyclophosphazotria obtained at the nerve stage was washed by heating with stirring with a ten-fold but by weight amount of 18% hydrochloric acid. Treatment was conducted at 60 ° C for 3 hours. During the saponification process, the resinous product went into solution.

At the end of the saponification, the solution was cooled and treated with a 25% potassium hydroxide solution. The light s.preen resinous product released at neutralization was washed with water at 40 ° C until neutral and dried in a vacuum oven. The resulting product, which crystallizes upon standing, according to the elementary analysis and the IR spectrum, was identified as tetraphenoxy-α-ankyloxycyclophosphazotriene, m.p. 144- 148 ° C, yield 69-73% (from theory), bat, and output 65%.

Found,%: C 59.35; 59.18; H 4.38; 4.25; N 9.15; 9.48.

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Calculated,%: C 59.75; H 4.46; N 9.68.

Example 2. A mixture of 17.34 g (0.03 mol) of tetraphenoxydichlorocyclophosphazotriene, 9.1 g (0.06 mol) of α -oxyacetanilide and 3.63 g (0.06 mol) of solid potassium hydroxide in 100 ml of xylene was stirred in a flask , equipped with a Dean-Stark trap cooler, at the boiling point of the solvent for 8 hours. The water evolving from the reaction was distilled off and collected in a trap. At the end of the reaction, the precipitate of potassium chloride was filtered from the cooled xylene solution, evaporated to dryness in vacuum (20-30 mm Hg). After cooling, the residue was a gummy mass of light brown in color, slowly crystallizing on standing. Yield 73-78%. According to the results of elementary analysis, the obtained product was identified as tetraphenoxy- (p-acetanyloxy) -cyclophosphazotriene. Found,%: C 59.05; 59.42; H 4.28; 4.35; N 8.12; 8.01.

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Calculated,%: C 59.48; H 4.49; N 8.67.

The resulting product was processed further as described in example 1.

After saponification, a resinous gum forms slowly crystallizing on standing.

brownish-lilac substance, so pl.

144-148 ° C, yield 69-73%; common outlet

45%:

Found,%: C 58.93; 59.12; H 4.87; 4.55; N 9.18; 9.33.

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Calculated,%: C 59.75; H 4.46; N 9.68.

Subject invention

Claims (2)

1. A method for producing tetraphenoxy-ananyloxycyclophosphazotriene, characterized by i eu, that tetraphenoxydichlorocyclophosphazotriene is treated with an alkali metal β-acetamidophenol in an organic solvent, such as pyridine, when heated, followed by saponification of the resulting compound in the presence of a mineral or organic acid, for example, and isolation of the target product by known techniques. 2. A method according to claim 1, characterized in that the process is carried out at a temperature of 50-150 ° C.