Preparation and properties of bromochlorofluorophosphine and improved synthesis for dimethylaminochlorofluorophosphine and dimethylaminbromofluorophosphine

Montemayor, R. G.; Parry, R. W.

doi:10.1021/ic50128a057

Cited by 11 publications

(2 citation statements)

References 2 publications

(2 reference statements)

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“…While the cleavage of P−N single bonds by haloacids is well documented the generation of a P−F bond in this manner has not been reported. , The reaction of [Cr(CO) 5 (P{NEt 2 } 3 )] with trimethyloxonium tetrafluoroborate produces [Cr(CO) 5 (PF{NEt 2 } 2 )] and only monofluorination is observed . A related conversion of [Fe(CO) 4 (PF 2 NEt 2 )] to [Fe(CO) 4 (PF 2 Cl)] using hydrogen chloride gas and of PF 2 NMe 2 to PF 2 X using anhydrous HX (X = Cl, Br, I) has been reported. , Kemmitt et al have also investigated the protonolysis of a number of metal complexes of dialkylaminophosphine ligands .…”

Section: Resultsmentioning

confidence: 99%

Synthesis and Characterization of the Trihalophosphine Compounds of Ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the Related PF₂(NMe₂) and P(NMe₂)₃Compounds; Multinuclear NMR Spectroscopy and the X-ray Single Crystal Structures of [RuBr₂(η⁶-cymene)(PF₃)], [RuBr₂(η⁶-cymene)(PF₂{NMe₂})], and [RuI₂(η⁶-cymene)(P{NMe
Boshaala
¹
,
Simpson
²
,
Autschbach
³

et al. 2008
Inorg. Chem.
14
2
12
0
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Treatment of the dimers [RuX2(eta(6)-cymene)]2 with PF3 in hot heptane produces the compounds [RuX2(eta(6)-cymene)(PF3)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX2(eta(6)-cymene)(PF2{NMe2})] and [RuX2(eta(6)-cymene)(P{NMe2}3)]. Reaction of the dimers [RuX2(eta(6)-cymene)]2 with PCl3 and PBr3 proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. (1)H, (13)C, (31)P, and (19)F NMR spectra have been obtained where appropriate together with ((1)H-(1)H) correlation spectroscopy (COSY) and ((13)C-(1)H)-HETCORR spectra of selected compounds. The variation of (1)J((31)P-(19)F) with the nature of the auxiliary ligand (X) in the PF3 and PF2(NMe2) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr2(eta(6)-cymene)(PF3)] has been determined at 223 K and those of [RuBr2(eta(6)-cymene)(PF2{NMe2})] and [RuI2(eta(6)-cymene)(P{NMe2}3)] at 294 K.

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Section: Resultsmentioning

confidence: 99%

Synthesis and Characterization of the Trihalophosphine Compounds of Ruthenium [RuX₂(η⁶-cymene)(PY₃)] (X = Cl, Br, Y = F, Cl, Br) and the Related PF₂(NMe₂) and P(NMe₂)₃Compounds; Multinuclear NMR Spectroscopy and the X-ray Single Crystal Structures of [RuBr₂(η⁶-cymene)(PF₃)], [RuBr₂(η⁶-cymene)(PF₂{NMe₂})], and [RuI₂(η⁶-cymene)(P{NMe
Boshaala
¹
,
Simpson
²
,
Autschbach
³

et al. 2008
Inorg. Chem.
14
2
12
0
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“…FP(NMe2)2 setzt sich mit HCl bzw. HBr zunächst zuMe2NPFHal um, und Me2NPClF reagiert mit HBr schheßlich zum PBrClF [6]. Durch P-NSpaltungsreaktionen gelangt man außerdem auf bequeme Weise zu Halogenophosphanen, die sonst nur auf Umwegen oder mit schlechteren Ausbeuten gewonnen werden können: Me2PCl [7], R2PC1 [8] und J-BuMePCl [9] sind dafür beispielhaft.…”

unclassified

Die Stabilisierung von P(NH₂)Hal₂ (Hal = Cl, Br, I) und P(NHMe)₂Cl als Komplexliganden / The Stabilisation of P(NH₂)Hal₂ (Hal = Cl, Br, I) and P(NHMe)₂Cl as Complex Ligands

Maisch

1982

Zeitschrift Für Naturforschung B

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The phosphanes P(NH2)Hal2 and P(NHMe)2Cl are stabilised as ligands in (CO)5MoP(NH2)Hal2 [Hal = Cl (2), Br (3), I (4)] and (CO)5MoP(NHMe)2Cl (10) by reactions of (CO)5MoP(NH2)3 (1) with HHal or of (CO)5MoP(NHMe)3 (8) with HCl, respectively. 4 decomposes at room temperature and reacts with t-BuNH2 to give, (CO)5MOP(NH-t-BU)2NH2 (6). 1 and HI form (CO)5MoPI3. 3 can also be prepared from 2 with HBr, 4 from 2 and 3 with HBr and HI, respectively. The reactions of 2-4 with NR3 produce polymers, whereas the reaction of 3 with pyridine leads to (CO)5MoNC5H5. The mixtures (CO)5MoP(NHMe)Br2/(CO)5MoPBr3 and (CO)5MoP(NH-i-Pr)2Cl/(CO)5MoP(NH-i-Pr)Cl2 are isolated from reactions of 8 with HBr and of 9 with HI, and 9 reacts with HBr to give (CO)5MoPBr3. (CO)5MoP(NHMe)I2 is formed in small amounts by the reaction of 8 with HI, the main product is an insoluble solid, which is probably the impure intermediate [(CO)5MoP(NHMe)(NH2Me)2]2+2I-. Reaction of 10 with NEt3 leads to the formation of the dinuclear complex 12 in which the new diazadiphosphetidine [MeNHP-NMe]2 functions as a bridging ligand between two (CO)5Mo units.

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In Noncyclic Species

Krannich¹

1988

Inorganic Reactions and Methods

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Preparation and properties of bromochlorofluorophosphine and improved synthesis for dimethylaminochlorofluorophosphine and dimethylaminbromofluorophosphine

Cited by 11 publications

References 2 publications

Die Stabilisierung von P(NH₂)Hal₂ (Hal = Cl, Br, I) und P(NHMe)₂Cl als Komplexliganden / The Stabilisation of P(NH₂)Hal₂ (Hal = Cl, Br, I) and P(NHMe)₂Cl as Complex Ligands

In Noncyclic Species

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Preparation and properties of bromochlorofluorophosphine and improved synthesis for dimethylaminochlorofluorophosphine and dimethylaminbromofluorophosphine

Cited by 11 publications

References 2 publications

Die Stabilisierung von P(NH2)Hal2 (Hal = Cl, Br, I) und P(NHMe)2Cl als Komplexliganden / The Stabilisation of P(NH2)Hal2 (Hal = Cl, Br, I) and P(NHMe)2Cl as Complex Ligands

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Die Stabilisierung von P(NH₂)Hal₂ (Hal = Cl, Br, I) und P(NHMe)₂Cl als Komplexliganden / The Stabilisation of P(NH₂)Hal₂ (Hal = Cl, Br, I) and P(NHMe)₂Cl as Complex Ligands