“…In the P-H coupled, 31 P NMR spectrum, a broad singlet and doublet is observed confirming assignment of these two resonances to the tertiary and secondary phosphines respectively ( 2 J P-P is not well resolved in these spectra, as is the case for other 31 P NMR spectra described below). Satisfactory 1 H and 13 C NMR spectra and analytical data are consistent with the formulation. The molecular cation (m/z = 447 amu) was observed in the mass spectrum as was the P-H stretch in the IR spectrum (m P-H 2322 cm −1 ).…”
Section: Results and Discussion 12-diphosphinobenzene Iron Template R...supporting
confidence: 67%
“…Analytical data and the 1 H and 13 C{ 1 H} NMR spectra are consistent with the structure of the macrocyclic complex (g 5 -pentamethylcyclopentadienyl)[meso-5 -vinyl -2,5,8 -triphosphabicyclo - [7.4.0]trideca-9(1),10,12-triene]iron(II) hexafluorophosphate (5a). The 1 H NMR spectrum clearly shows the separate components of 5a in the anticipated intensity ratios.…”
Section: Results and Discussion 12-diphosphinobenzene Iron Template R...supporting
confidence: 62%
“…The second signal is assigned to the other secondary phosphine and the third as the tertiary phosphine (doublet, 1 J P-H = 352 Hz, and singlet in the 31 P NMR spectrum respectively), both appearing as double doublets (J BC = 6.6 Hz). As well as satisfactory analytical data, 5d is also characterised by its molecular ion in the mass spectrum (m/z = 475 amu), m P-H in the IR spectrum (2327 cm −1 ) and the 1 H and 13 C NMR data are consistent with the proposed structure.…”
Section: Functionalised Macrocycles: On the Backbonesupporting
[eta(5)-Cp(R)Fe(CH3CN)(1,2-diphosphinobenzene)]+ complexes are readily formed from [eta(5)-Cp(R)FeL3]+ salts and act as template precursors for the intramolecular hydrophosphination of co-ordinated trivinylphosphine with 1,2-diphosphinobenzenes. This sequence constitutes a versatile synthetic route to a new class of co-ordinated triphosphacyclononanes bearing a rigid o-phenylene backbone link. The efficiency of the synthesis depends markedly upon the nature of the Cp(R) ligand. The new secondary phosphine macrocycles prepared by this route are readily alkylated to tritertiary triphosphine macrocycles bearing alkyl and pendant functions.
“…In the P-H coupled, 31 P NMR spectrum, a broad singlet and doublet is observed confirming assignment of these two resonances to the tertiary and secondary phosphines respectively ( 2 J P-P is not well resolved in these spectra, as is the case for other 31 P NMR spectra described below). Satisfactory 1 H and 13 C NMR spectra and analytical data are consistent with the formulation. The molecular cation (m/z = 447 amu) was observed in the mass spectrum as was the P-H stretch in the IR spectrum (m P-H 2322 cm −1 ).…”
Section: Results and Discussion 12-diphosphinobenzene Iron Template R...supporting
confidence: 67%
“…Analytical data and the 1 H and 13 C{ 1 H} NMR spectra are consistent with the structure of the macrocyclic complex (g 5 -pentamethylcyclopentadienyl)[meso-5 -vinyl -2,5,8 -triphosphabicyclo - [7.4.0]trideca-9(1),10,12-triene]iron(II) hexafluorophosphate (5a). The 1 H NMR spectrum clearly shows the separate components of 5a in the anticipated intensity ratios.…”
Section: Results and Discussion 12-diphosphinobenzene Iron Template R...supporting
confidence: 62%
“…The second signal is assigned to the other secondary phosphine and the third as the tertiary phosphine (doublet, 1 J P-H = 352 Hz, and singlet in the 31 P NMR spectrum respectively), both appearing as double doublets (J BC = 6.6 Hz). As well as satisfactory analytical data, 5d is also characterised by its molecular ion in the mass spectrum (m/z = 475 amu), m P-H in the IR spectrum (2327 cm −1 ) and the 1 H and 13 C NMR data are consistent with the proposed structure.…”
Section: Functionalised Macrocycles: On the Backbonesupporting
[eta(5)-Cp(R)Fe(CH3CN)(1,2-diphosphinobenzene)]+ complexes are readily formed from [eta(5)-Cp(R)FeL3]+ salts and act as template precursors for the intramolecular hydrophosphination of co-ordinated trivinylphosphine with 1,2-diphosphinobenzenes. This sequence constitutes a versatile synthetic route to a new class of co-ordinated triphosphacyclononanes bearing a rigid o-phenylene backbone link. The efficiency of the synthesis depends markedly upon the nature of the Cp(R) ligand. The new secondary phosphine macrocycles prepared by this route are readily alkylated to tritertiary triphosphine macrocycles bearing alkyl and pendant functions.
Alcohols Q 0230Allylation of Aldehydes and Imines: Promoted by Reuseable Polymer-Supported Sulfonamide of N-Glycine. -The reaction affords the products in high yields and most of the -SnBu3 residue is recovered as Bu3SnCl. The polymeric promoter can be reused at least five times without loss of activity. The method is further used for the preparation of bioactive natural products L-733,060 (XVII) and CP-99,994 (XVIII).
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