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inquiryphosphorus pentachloride
ammonium chloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
(NPCl2)8
C
octachlorocyclotetraphosphazene
E
pentakisphosphorus nitride dichloride
F
hexakisphosphorus nitride dichloride
G
heptakisphosphorus nitride dichloride
Conditions | Yield |
---|---|
In chlorobenzene Schlenk technique; Reflux; | A 64% B 6% C 5% D 2% E 16% F 16% G 13% |
phosphorus pentachloride
ammonium chloride
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With pyridine In 1,1,2,2-tetrachloroethane at 130℃; for 8h; | 58.2% |
phosphorus pentachloride
ammonia
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In tetrachloromethane pptn. of NH4Cl from a soln. of 3 g PCl5 in 1000 ml CCl4 half-saturated with gaseous NH3 at -3 °C; soln. contains (PNCl2)3 and (PNCl2)4;; evapn. of the mother liquor, fractional crystn. from toluene;; | |
In tetrachloromethane pptn. of NH4Cl from a soln. of 3 g PCl5 in 1000 ml CCl4 half-saturated with gaseous NH3 at -3 °C; soln. contains (PNCl2)3 and (PNCl2)4;; evapn. of the mother liquor, fractional crystn. from toluene;; |
chlorine
phosphorus trichloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
C
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In further solvent(s) dissolving PCl3 distd. under N2 in benzyl chloride distd. under N2; addn. of NH4Cl dryed in vac. and passing in the corresponding amount of Cl2; heating in a stream of N2 at 130 °C; removal of formed HCl by a stream of N2;; filtration, distg. off the solvent at 40 °C and 0.5 Torr; recrystn. from petroleum ether; product contains small amounts of higher polymers;; |
chlorine
phosphorus trichloride
A
hydrogenchloride
B
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
D
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In further solvent(s) dissolving PCl3 distd. under N2 in (CHCl2)2 distd. under N2; addn. of NH4Cl dryed in vac. and passing in the corresponding amount of Cl2; heating in a stream of N2 at 130 °C; removal of formed HCl by a stream of N2;; filtration, distg. off the solvent at 40 °C and 0.5 Torr; recrystn. from petroleum ether; products (NPCl2)3, (NPCl2)4 and a small amount of oily polymers;; | |
In chlorobenzene dissolving PCl3 distd. under N2 in C6H5Cl distd. under N2; addn. of NH4Cl dryed in vac. and passing in the corresponding amount of Cl2; heating in a stream of N2 at 130 °C; removal of formed HCl by a stream of N2;; filtration, distg. off the solvent at 40 °C and 0.5 Torr; recrystn. from petroleum ether; product contains small amounts of higher polymers;; | |
In further solvent(s) dissolving PCl3 distd. under N2 in (CHCl2)2 distd. under N2; addn. of NH4Cl dryed in vac. and passing in the corresponding amount of Cl2; heating in a stream of N2 at 130 °C; removal of formed HCl by a stream of N2;; filtration, distg. off the solvent at 40 °C and 0.5 Torr; recrystn. from petroleum ether; yield 35-40 %, product contains small amounts of higher polymers;; | A n/a B 35-40 C n/a D n/a |
phosphorus pentachloride
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In further solvent(s) react. of PCl5 with NH4Cl in (CHCl2)2;; recrystn. of the fraction containing (NPCl2)4 (180-187 °C at 10 Torr) from ethyl ether under discoloration of coal;; | |
In further solvent(s) react. of PCl5 with NH4Cl in (CHCl2)2;; recrystn. of the fraction containing (NPCl2)4 (180-187 °C at 10 Torr) from ethyl ether under discoloration of coal;; |
phosphorus pentachloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
C
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In not given react. of 400 g PCl5 with 120 g NH4Cl in an inert solvent;; sucking off the formed mass, washing with ice-cold C6H6; fractional distn.; yield 50 % (NPCl2)3, 25 % (NPCl2)4 and 25 % higher polymers;; |
phosphorus pentachloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In not given react. of 400 g PCl5 with 120 g NH4Cl in an inert solvent;; sucking off the formed mass, washing with ice-cold C6H6; fractional distn.; yield 75 g (NPCl2)3, 25 g (NPCl2)4;; | |
In not given react. of PCl5 with NH4Cl;; fractionation at 185-190 °C and 13 Torr; fraction contains 10 % (NPCl2)3;; | |
In not given react. of PCl5 with NH4Cl;; fractionation at 185-190 °C and 13 Torr; fraction contains 10 % (NPCl2)3;; | |
In further solvent(s) react. of finely divided NH4Cl and PCl5 in refluxing sym-tetrachloroethane; fractional crystn. from glacial acetic acid, cold benzene and conc. H2SO4; |
Conditions | Yield |
---|---|
In not given react. of (Cl3PNPCl3)Cl with NH4Cl;; | |
In not given react. of (Cl3PNPCl3)Cl with NH4Cl;; |
lithium azide
trichloro(o-phenylenedioxy)phosphorane
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
hexaazido cyclotriphosphazene
C
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In nitrobenzene not isolated, detected by NMR; |
lithium azide
PCl5(C5H5N)
A
1,1,3,3,5,5,7,7-octaazido-cyclo-tetraphosphazene
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In dichloromethane byproducts: PCl4(N3)(pyridine); detected by NMR; |
2,4-dichloro-1,3-bis(dichlorophosphoryl)-2,4-dioxocyclodiphosph(V)azane
phosphorus pentachloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
dichlorophosphinylphosphorimidic trichloride
C
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In trichlorophosphate byproducts: Cl2(O)P(NPCl2)5Cl; under reflux; treatment of the crude product with n-heptane, products identified in the sol. and in the insol. phase with NMR spectroscopy; |
phosphorus trichloride
A
hydrogenchloride
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In not given reaction with an equimolar amount of PCl3 under formation of P4N4Cl8 and evolution of 2 mol HCl;; | |
In not given reaction with an equimolar amount of PCl3 under formation of P4N4Cl8 and evolution of 2 mol HCl;; |
tris(trimethylsilyl)amine
phosphorus pentachloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
C
pentakisphosphorus nitride dichloride
D
hexakisphosphorus nitride dichloride
Conditions | Yield |
---|---|
In dichloromethane byproducts: high oligomers; inert atmosphere; dropwise addn. of 1 equiv. PCl5 to amine at reflux, refluxing for 8 h; distn.; product mixt. not sepd., detd. by (31)P-NMR spectroscopy; |
phosphorus pentachloride
ammonia
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In tetrachloromethane incomplete satn. of a soln. of PCl5 in CCl4 with gaseous NH3;; | |
In tetrachloromethane |
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
byproducts: HCl; decomposition upon warming; |
phosphorus pentachloride
ammonium chloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
C
pentakisphosphorus nitride dichloride
Conditions | Yield |
---|---|
zinc(II) oxide In 1,2-dichloro-benzene at 177℃; for 6.01667h; Product distribution / selectivity; |
trichloro(trimethylsilyl)phosphoranimine
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With [PCl2(NP(C6H5)3)2]Cl In dichloromethane (N2); a soln. of Si compd. added dropwise to a soln. of PCl2(NP(C6H5)3)2Cl, stirred for 24 h at 25°C; not isolated, detected by NMR; |
phosphorus pentachloride
A
hydrogenchloride
B
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
C
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
In further solvent(s) NH4Cl reacted with PCl5 in 1,1,2,2-tetrachloroethane according to L. G. Lund, N. L. Paddock, J. E. Proctor, H. T. Searle, Journal of the Chemical Society (1960) 2542; vac. distilled on Vigreux column; |
phosphorus pentachloride
ammonium chloride
A
2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
B
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With zinc(II) chloride In chlorobenzene for 40h; Reflux; | A 70 %Chromat. B 19 %Chromat. |
Conditions | Yield |
---|---|
With sodium hydride In tetrahydrofuran at -20 - 20℃; | 90% |
With sodium hydride In tetrahydrofuran at -20 - 20℃; for 48h; | 90% |
Conditions | Yield |
---|---|
With sodium hydride In tetrahydrofuran at 20℃; for 3h; Inert atmosphere; | 87% |
octachlorocyclotetraphosphazene
octafluorophosphazene
Conditions | Yield |
---|---|
In neat (no solvent) react. at 280-350 °C; complete react. after 2 1/2 h; passing through N2 at the end of the react.;; distn. off the product or removal of product with N2;; | 84.5% |
In neat (no solvent) react. at 280-350 °C; complete react. after 2 1/2 h; passing through N2 at the end of the react.;; distn. off the product or removal of product with N2;; | 84.5% |
C6H3(OH)[COHNC3H6Si(CH3)2C5H4FeC5H3[P(C6H5)2]CH(CH3)P(C6H11)2]2
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With sodium In 1,4-dioxane; methanol react. of phenol with Na (1 h at 60°C), then with N4P4Cl8 (16 h); column chromy.; | 83% |
Conditions | Yield |
---|---|
Stage #1: octachlorocyclotetraphosphazene; (R,S)-2,2-dimethyl-1,3-dioxolane-4-methanol With sodium hydride In tetrahydrofuran; water; mineral oil at 20℃; for 24h; Stage #2: With octachlorocyclotetraphosphazene In tetrahydrofuran; water; mineral oil at 30℃; for 24h; | 81.2% |
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran for 24h; Inert atmosphere; Reflux; | 80% |
Conditions | Yield |
---|---|
In neat (no solvent) condensation of liquid SO2 on a mixt. of (NPCl2)4 and KF; heating at 98-100 °C for 22 days;; removal of an excess of SO2; fractionation;; | 77% |
In neat (no solvent) heating (NPCl2)4 with a 50 % excess of KF and less than the stoichiometric amount of SO2 at 100 °C in an autoclave for a few days on stirring;; | |
In neat (no solvent) heating (NPCl2)4 with a 50 % excess of KF and less than the stoichiometric amount of SO2 at 100 °C in an autoclave for a few days on stirring;; |
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran for 24h; Inert atmosphere; Reflux; | 77% |
potassium fluorosulphinate
octachlorocyclotetraphosphazene
A
octafluorophosphazene
B
sulfur dioxide
Conditions | Yield |
---|---|
In nitrobenzene heating a soln. of (NPCl2)4 in C6H5NO2 with solid 90 % KSO2F on refluxing; react. starting at 80. degree.C under evolution of gas;; condensation of (NPCl2)3 and formed SO2 on cooling with ice-water; distn. in vac.;; | A 75% B n/a |
In nitrobenzene heating a soln. of (NPCl2)4 in C6H5NO2 with solid 90 % KSO2F on refluxing; react. starting at 80. degree.C under evolution of gas;; condensation of (NPCl2)3 and formed SO2 on cooling with ice-water; distn. in vac.;; | A 75% B n/a |
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at 20℃; for 4h; Inert atmosphere; Cooling with ice; | 75% |
2-azidoethanol
octachlorocyclotetraphosphazene
2,2,4,4,6,6,8,8-octakis-(2′-azido-1′-ethoxy)-cyclotetraphosphazatetraene
Conditions | Yield |
---|---|
With sodium hydride In tetrahydrofuran at 20℃; for 24h; Inert atmosphere; Cooling with ice; | 70% |
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at 20℃; for 4h; Inert atmosphere; Cooling with ice; | 70% |
N,N'-bis(2-hydroxybenzyl)ethylenediamine
octachlorocyclotetraphosphazene
B
C16H16Cl4N6O2P4
Conditions | Yield |
---|---|
Stage #1: N,N'-bis(2-hydroxybenzyl)ethylenediamine With potassium carbonate In tetrahydrofuran for 4h; Inert atmosphere; Reflux; Stage #2: octachlorocyclotetraphosphazene With triethylamine In tetrahydrofuran at -10 - 20℃; for 21h; | A 69% B 22% |
octachlorocyclotetraphosphazene
1-amino-naphthalene
octakis(1-napthylamino)cyclotetraphosphazene
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran for 24h; Inert atmosphere; Reflux; | 63% |
octachlorocyclotetraphosphazene
N,N'-bis(2-hydroxybenzyl)-1,3-diaminopropane
B
C17H18Cl4N6O2P4
Conditions | Yield |
---|---|
Stage #1: N,N'-bis(2-hydroxybenzyl)-1,3-diaminopropane With potassium carbonate In tetrahydrofuran for 4h; Inert atmosphere; Reflux; Stage #2: octachlorocyclotetraphosphazene With triethylamine In tetrahydrofuran at -10 - 20℃; for 21h; | A 63% B 29% |
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at 20℃; for 4h; Inert atmosphere; Cooling with ice; | 63% |
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at -10 - 20℃; for 74h; Inert atmosphere; | A 6% B 62% C 18% |
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With caesium carbonate In tetrahydrofuran at 20℃; for 72h; Inert atmosphere; Cooling with ice; | 57% |
Conditions | Yield |
---|---|
With NEt3 In tetrahydrofuran byproducts: NEt3*HCl; Ar atm.; stoichiometric ratio, cooling (-78°C), stirring (overnigh); filtn., evapn. (vac.), extraction (CH2Cl2), chromatography (SiO2, CH2Cl2); | 53% |
Conditions | Yield |
---|---|
Stage #1: octachlorocyclotetraphosphazene; diethylene glycol In dichloromethane at 20℃; for 2h; Stage #2: With pyridine In dichloromethane at 20℃; for 16h; Cooling with ice; | A 24.6% B 24.25% C 48.5% |
Conditions | Yield |
---|---|
With NEt3 In tetrahydrofuran byproducts: NEt3*HCl; Ar atm.; equimolar ratio, cooling (-78°C), stirring (overnight, room temp.); concn. (vac.), chromatography (SiO2/CH2Cl2); | 47% |
octachlorocyclotetraphosphazene
[Fe(C5H4S)2P4N4Cl6]
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: LiCl; Ar atm.; stoichiometric ratio, cooling (-78°C), stirring (overnigh); filtn., evapn. (vac.), extraction (CH2Cl2), chromatography (SiO2, CH2Cl2); | 45% |
N'-(1-ferrocenylmethyl)-N-methyl-ethylenediamine
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at -5 - 20℃; for 72h; Inert atmosphere; | 45% |
octachlorocyclotetraphosphazene
tert-butylamine
tert-Butyl-(2,4,4,6,6,8,8-heptachloro-2λ5,4λ5,6λ5,8λ5-[1,3,5,7,2,4,6,8]tetrazatetraphosphocin-2-yl)-amine
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at 20℃; for 4h; Inert atmosphere; Cooling with ice; | 43% |
octachlorocyclotetraphosphazene
6-amino-3,4-benzodioxane
B
C16H16Cl6N6O4P4
C
C8H8Cl7N5O2P4
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at 20℃; for 48h; Inert atmosphere; | A 25% B 13% C 42% |
octachlorocyclotetraphosphazene
Conditions | Yield |
---|---|
With triethylamine In tetrahydrofuran at -5 - 20℃; for 72h; Inert atmosphere; | 42% |
octachlorocyclotetraphosphazene
[Fe(C5H4Se)2P4N4Cl6]
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: LiCl; Ar atm.; stoichiometric ratio, cooling (-78°C), stirring (overnigh); filtn., evapn. (vac.), extraction (CH2Cl2), chromatography (SiO2, CH2Cl2); | 41% |
Conditions | Yield |
---|---|
Stage #1: octachlorocyclotetraphosphazene; diethylene glycol In dichloromethane at 20℃; for 2h; Stage #2: With pyridine In dichloromethane at 20℃; for 24h; Cooling with ice; | A 15.3% B 17.1% C 40.8% D 22.2% |
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