[Tris(dimethylamino)phosphonioamino]tris[tris...

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

Reexamination Certificate

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Reexamination Certificate

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06177593

ABSTRACT:

BACKGROUND OF THE INVENTION
a) Field of the Invention
This invention relates to novel and useful [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride.
This compound is extremely useful as a raw material for tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide which is important as a polymerization catalyst for alkylene oxides.
This [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride is also an important compound upon extracting tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride as its hydrogen chloride addition compound in a water phase from a solution of the chloride in an organic solvent such as a reaction mixture containing the chloride.
Further, the present invention is also concerned with a process for preparing [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride and also with a process for extracting and separating tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride as [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride, the hydrogen chloride addition compound of the chloride, in a water phase from a solution of the chloride in an organic solvent.
Furthermore, this invention also pertains to a process for preparing tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide from an aqueous solution of [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride obtained by conducting extraction and separation as described above and also to a process for isolating the hydroxide as a solid.
Moreover, this invention also relates to a process for regenerating tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride from the aqueous solution of the dichloride and isolating the same as a solid.
b) Description of the Related Art
[Tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride is a compound absolutely unknown to date. Further, it has heretofore been totally unknown and undisclosed in any publication that, when tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride and hydrogen chloride are brought into contact with each other, [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride as the hydrogen chloride addition product of the chloride is formed.
Needless to say, there is absolutely no precedent case of practice of the process for extracting and separating tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride as [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride, the hydrogen chloride addition compound of the chloride, in a water phase from a solution of the chloride in an organic solvent, the process for preparing tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide from an aqueous solution of [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride obtained by conducting extraction and separation as described above, or the process for isolating the hydroxide as a solid; and no publications suggestive of such processes.
Furthermore, no process is known at all and is suggested in any publication for regenerating tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride from the aqueous solution of the dichloride and isolating the same as a solid.
SUMMARY OF THE INVENTION
A first object of the present invention is to provide a raw material which upon preparation of tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide important as a polymerization catalyst for alkylene oxides, can easily afford the hydroxide by an extremely convenient process.
A second object of the present invention is to provide the convenient preparation process for the raw material.
Tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride is an important compound as a raw material for tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide.
To convert the chloride into tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide, it is desired to use the chloride in the form of an aqueous solution.
The chloride is usually obtained by a reaction of phosphorus pentachloride and iminotris(dimethylamino)phosphorane in an organic solvent, and is dissolved extremely well in the organic solvent. This has made it practically impossible to transfer the chloride into a water phase by the convenient method, namely extraction in water. It is therefore extremely difficult to separate the chloride by this method.
There is accordingly a long standing desire for the development of an effective separation method.
Namely, a third object of the present invention is to provide an extraction and separation process of tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride by conveniently transferring the chloride into a water phase from a solution of the chloride in an organic solvent.
A fourth object of the present invention is to provide a process for conveniently and easily preparing tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide from an aqueous solution containing the chloride so extracted and separated and also a process for isolating the hydroxide as a solid.
Moreover, a fifth object of the present invention is to provide a process for regenerating and isolating as a solid tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride from the aqueous solution containing the chloride so extracted and separated.
The present inventors have proceeded with an extensive investigation to achieve the above-described objects. As a result, a novel compound capable of extremely conveniently and easily affording tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride, namely [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride has been found and, moreover, a process has also been found for its easy preparation.
Inherently, tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride is soluble up to 4 wt. % or so in water. Nevertheless, attempts to extract and separate the chloride from a solution of the chloride in an organic solvent all resulted in failure due to its high solubility in the organic solvent.
It has however been surprisingly found that extraction with an aqueous solution of hydrogen chloride in place of pure water converts the chloride into its hydrogen chloride addition compound, i.e., [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride, leading to a substantial increase in the solubility in water and also to a significant decrease in the solubility in an organic solvent so that the dichloride can be transferred into a water phase with extremely high efficiency. Here, the organic solvent must be immiscible with water.
It has also been found that the hydrogen chloride addition compound of tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride, namely [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride so extracted and separated can be converted into tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide by simply bringing its aqueous solution into contact with an OH

-form ion exchange resin.
It has also been found that neutrali

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