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New Products from PCl₃, P(NMe₂)₃, and AlCl₃^†^‡

Corresponding Author

Prof. Dr. Alfred Schmidpeter

Institut für Anorganische Chemie der Universität, Meiserstrasse 1, D-8000 München 2 (FRG)

Institut für Anorganische Chemie der Universität, Meiserstrasse 1, D-8000 München 2 (FRG)Search for more papers by this author

Dr. Siegfried Lochschmidt,

Dr. Siegfried Lochschmidt

Institut für Anorganische Chemie der Universität, Meiserstrasse 1, D-8000 München 2 (FRG)

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Prof. Dr. Alfred Schmidpeter,

Corresponding Author

Prof. Dr. Alfred Schmidpeter

Institut für Anorganische Chemie der Universität, Meiserstrasse 1, D-8000 München 2 (FRG)

Institut für Anorganische Chemie der Universität, Meiserstrasse 1, D-8000 München 2 (FRG)Search for more papers by this author

Dr. Siegfried Lochschmidt,

Dr. Siegfried Lochschmidt

Institut für Anorganische Chemie der Universität, Meiserstrasse 1, D-8000 München 2 (FRG)

Search for more papers by this author

First published: March 1986

https://doi.org/10.1002/anie.198602531

Citations: 37

^†

This work was supported by the Deutsche Forschungsgemeinschaft and the Fonds der Chemischen Industrie.

^‡

Dedicated to Professor Rolf Appel on the occasion of his 65th birthday

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Exploitation of an old and frequently studied reaction (to obtain new compounds) has proven successful with the system PCl₃/P(NMe₂)₃/AlCl₃. Depending on the sequence in which the reaction partners are allowed to react with each other, different products are formed. The most interesting new products are the diphosphoniodiphosphirane ion 1 (the CH₂ group comes from the solvent CH₂Cl₂) and the cyclotetraphosphane ion 2.

References

1 J. R. Van Wazer, L. Maier, J. Am. Chem. Soc. 86 (1964) 811.
10.1021/ja01059a013
CAS Web of Science® Google Scholar
2 C. W. Schultz, R. W. Parry, Inorg. Chem. 15 (1976) 3046.
10.1021/ic50166a022
CAS Web of Science® Google Scholar
3 A. Schmidpeter, S. Lochschmidt, W. S. Sheldrick, Angew. Chem. 97 (1985) 214;
10.1002/ange.19850970313
CAS Google Scholar
Angew. Chem. Int. Ed. Engl. 24 (1985) 226.
10.1002/anie.198502261
Web of Science® Google Scholar
4 ³¹P-NMR of 6 (AB₂): δ_A = −142, δ_B = +70; J_AB = 290 Hz.
Google Scholar
5 ³¹P-NMR of 7 (AB₂): δ_A = −131, δ_B = +63; J_AB = 270 Hz, ¹J_PH = 241 Hz.
Google Scholar
6 A. Schmidpeter, S. Lochschmidt, K. Karaghiosoff, W. S. Sheldrick, J. Chem. Soc. Chem. Commun. 1985, 1447.
Google Scholar
7 ³¹P-NMR of 8 (AA′BB′):δ_A: = −198 (ring phosphorus), δ_B = +67 (phosphonio group); J_AA = ∓120 Hz, J _AB = ∓312 Hz, J_AB = ±47 Hz, J_BB = ±48 Hz. An X-ray structure investigation has been carried out on a differently substituted diphosphoniodiphosphirane.
Google Scholar
S. Lochschmidt, G. Müller, B. Huber, A. Schmidpeter, Z. Naturforsch. B41 (1986), in press.
Google Scholar
8 A. Schmidpeter, S. Lochschmidt, A. Willhalm, Angew. Chem. 95 (1983) 561;
10.1002/ange.19830950713
CAS Google Scholar
Angew. Chem. Int. Ed. Engl. 22 (1983) 545;
10.1002/anie.198305451
Web of Science® Google Scholar
Angew. Chem. Suppl. 1983, 710.
Google Scholar
9 M. Baudler, F. Saykowski, Z. Naturforsch. B33 (1978) 1208;
Google Scholar
M. Baudler, G. Reuschenbach, Z. Anorg. Allg. Chem. 464 (1980) 9.
10.1002/zaac.19804640103
CAS Web of Science® Google Scholar
10 ³¹P-NMR of 9 (AA′BB′C₂): δ_A = −24 (phosphonio-substituted ring phosphorus), δ_C = ±18 (amino-substituted ring phosphorus, cf. [11]), δ_B = + 69 (phosphonio groups).
Google Scholar
11 R. B. King, N. D. Sadanani, P. M. Sundaram, Phosphorus Sulfur 18 (1983) 125.
10.1080/03086648308075983
CAS Web of Science® Google Scholar
12 Experimental procedure: 10: PCl₃ (0.78 mL, 8.4 mmol) was added with vigorous stirring to P(NMe₂)₃ (4.74 mL, 26.1 mmol) and NaBPh₄ (6.00 g, 17.4 mmol) in 120 mL of dimethoxyethane. After 2 h, the colorless precipitate was separated and extracted with 100 mL of CH₂Cl₂. After concentration of the extracts by a factor of ten, crystallization occurred to give 3.92g (69%) of 10: m.p. = 161°C; ¹H-NMR: δ = 2.76, J_PNCH = 10.7 Hz.–³¹P-NMR (AB₂): δ_A = −194, δ_B = +85; J_AB = 513Hz (cf.[3]).
Google Scholar

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Volume25, Issue3

March 1986

Pages 253-254

New Products from PCl₃, P(NMe₂)₃, and AlCl₃^†^‡

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New Products from PCl3, P(NMe2)3, and AlCl3†‡

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New Products from PCl₃, P(NMe₂)₃, and AlCl₃^†^‡