Preparation process of iminotris ( Dimethylamino) phosphorane

Organic compounds -- part of the class 532-570 series – Organic compounds – Amino nitrogen containing

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C07F 906

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060909803

ABSTRACT:
A process is provided for preparing iminotris(dimethylamino)phosphorane at high purity and high yield from aminotris(dimethylamino)phosphonium chloride. Aminotris(dimethylamino)phosphonium chloride is first reacted with an aqueous solution of the hydroxide of an alkali metal or alkaline earth metal in the presence of a solvent in which the chloride and hydroxide of the alkali metal or alkaline earth metal are sparingly soluble, whereby iminotris(dimethylamino)phosphorane is formed. After water is dissolved off at a temperature of 70.degree. C. or lower from the reaction mixture, solids are removed from the thus-concentrated reaction mixture by solid-liquid separation. The resultant mother liquor is then distilled to obtain iminotris(dimethylamino)phosphorane.

REFERENCES:
Koidan et al, "Some Properties of Phosphorimidic Triamides", Journal of General Chemistry USSR, vol. 52, No. 9, Feb. 20, 1983, pp. 1779-1787.
Chemical Abstracts, vol. 093, No. 8, Aug. 25, 1980, Columbus, Ohio, Abstract No. 087657, Marchenko et al, "Ammonolysis of Triamidohalophosphonium Halides".
Marchenko et al, "N''-unsubstituted Phosphorimidic Triamides", Journal of General Chemistry USSR, vol. 48, No. 12/2, Jun. 10, 1979, p. 2529.
Issleib et al, "Dimethylaminoiminophosphorane", Syn. Inorg. Metal-Org. Chem. (Simoai), 1973, vol. 3 (3), pp. 255-266.
Database WPI, Section Ch, Week 9903, Derwent Publications Ltd., London, GB, Class E11, AN 99-029065, Japanese Patent Publication No. 97-0338821, 1998.

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