Conditions | Yield |
---|---|
In neat (no solvent) drying mixt. of K2NbF7 and LiCl2 at 150°C, heating mixt. in inert gas atmosphere at 750°C for 1 h;; | 90% |
In neat (no solvent) drying mixt. of K2NbF7 and LiCl2 at 150°C, heating mixt. in inert gas atmosphere at 750°C for 1 h;; | 90% |
Conditions | Yield |
---|---|
In neat (no solvent) drying mixt. of K2NbF7 and CaCl2 at 150°C, heating mixt. in inert gas atmosphere at 750°C for 1 h;; | 90% |
In neat (no solvent) drying mixt. of K2NbF7 and CaCl2 at 150°C, heating mixt. in inert gas atmosphere at 750°C for 1 h;; | 90% |
potassium heptafluoroniobate(V)
magnesium chloride
niobium pentachloride
Conditions | Yield |
---|---|
In neat (no solvent) drying mixt. of K2NbF7 and MgCl2 at 150°C, heating mixt. in inert gas atmosphere at 750°C for 1 h;; | 90% |
In neat (no solvent) drying mixt. of K2NbF7 and MgCl2 at 150°C, heating mixt. in inert gas atmosphere at 750°C for 1 h;; | 90% |
phosphorus pentachloride
A
niobium pentachloride
B
tellurium tetrachloride
C
phosphorus trichloride
Conditions | Yield |
---|---|
In neat (no solvent) molar ratio niobium ditelluride/PCl5 1/8; heated in evacuated sealed ampoules for 2 h at 170°C, cooled; PCl3 removed in a vac. at 80°C, extd. with hot monoglyme, the residue dried in a vac.; NMR, mass spectra; | A n/a B n/a C 82% |
In neat (no solvent) molar ratio niobium ditelluride/PCl5 1/4; heated in evacuated sealed ampoules for 2 h at 170°C, cooled; PCl3 removed in a vac. at 80°C, extd. with hot monoglyme, the residue dried in a vac.; NMR, mass spectra; | A n/a B n/a C >99 |
Conditions | Yield |
---|---|
In neat (no solvent) NbOCl3 is chlorinated by COCl2 over coal heated to 350 - 600°C (most favourable results are achieved by use of active coal) to give NbCl5;; | |
In neat (no solvent) NbOCl3 is chlorinated by COCl2 over coal heated to 350 - 600°C (most favourable results are achieved by use of active coal) to give NbCl5;; |
Conditions | Yield |
---|---|
In neat (no solvent) at 280°C in sealed tube;; |
Conditions | Yield |
---|---|
With carbon monoxide In neat (no solvent) NbOCl3 is chlorinated by equimolar mixts. of CO and Cl2 or by COCl2 over coal heated to 350 - 600°C (most favourable results are achievedby use of active coal) to give NbCl5;; | |
With carbon monoxide In neat (no solvent) NbOCl3 is chlorinated by equimolar mixts. of CO and Cl2 or by COCl2 over coal heated to 350 - 600°C (most favourable results are achievedby use of active coal) to give NbCl5;; |
niobium pentachloride
Conditions | Yield |
---|---|
With Cl2 |
Conditions | Yield |
---|---|
In neat (no solvent) byproducts: H2; from Nb powder, 300-350°C, 1 h; | |
In neat (no solvent) byproducts: NbCl4; in stream of HCl at 300-900°C;; mixt. of products obtained; small amt. of NbCl4;; | |
In neat (no solvent) from granulated Nb, above 400°C; |
hydrogenchloride
C
niobium pentachloride
Conditions | Yield |
---|---|
In neat (no solvent) 800°C, in HCl flow; | A 0% B n/a C n/a |
In neat (no solvent) 800°C, in HCl flow; | A 0% B n/a C n/a |
Conditions | Yield |
---|---|
In neat (no solvent) byproducts: H2; from Nb powder, quenching; | |
In neat (no solvent) byproducts: H2; from Nb powder, quenching; |
Conditions | Yield |
---|---|
In neat (no solvent) at 180 - 190°C;; | |
In neat (no solvent) at 205°C;; | |
In neat (no solvent) from Nb powder,180-190°C; |
Conditions | Yield |
---|---|
In melt Kinetics; 550°C, conducting of Cl2 into the melt, sublimation of NbCl5; | |
In melt Kinetics; 550°C, conducting of Cl2 into the melt, sublimation of NbCl5; |
Conditions | Yield |
---|---|
With water In melt Kinetics; react. at 550-800°C, dissolution in H2O: Nb(IV)-oxide formed;parts of the reaction mixture sublimated: NbCl5, niobium oxichloride, NbCl3 formed; | |
With H2O In melt Kinetics; react. at 550-800°C, dissolution in H2O: Nb(IV)-oxide formed;parts of the reaction mixture sublimated: NbCl5, niobium oxichloride, NbCl3 formed; |
Conditions | Yield |
---|---|
In melt in PbCl2 melt at 550-800°C;; sublimate with 90 % NbCl5 and 10 % NbCl3;; | |
In melt byproducts: NbOCl3; 550-800°C;; sublimate contains 90 % NbCl5, 10 % NbCl3 impured with NbOCl3, melt contains Nb(V) and other oxidation states;; | |
In melt byproducts: NbOCl3; 550-800°C;; sublimate contains 90 % NbCl5, 10 % NbCl3 impured with NbOCl3, melt contains Nb(V) and other oxidation states;; |
Conditions | Yield |
---|---|
In melt Kinetics; 550-800°C, partial sublimation of Nb2O5; | |
In melt Kinetics; 550-800°C, partial sublimation of Nb2O5; |
Conditions | Yield |
---|---|
In melt in PbCl2 melt at 550°C and presence of Cl2;; nearly complete vapn. of Nb as NbCl5;; |
Conditions | Yield |
---|---|
In neat (no solvent, gas phase) thermal-sublimation column, Ar as carrier gas for SOCl2, heating (850°C, 20 min); drying the products over P2O5, elem. anal., product ratio depending on deposition temp.; |
Conditions | Yield |
---|---|
In neat (no solvent) in a sealed tube at 290°C;; | >99 |
In neat (no solvent) in a sealed tube at 290°C;; | >99 |
Conditions | Yield |
---|---|
In neat (no solvent) in stream of SOCl2 vapor at 300-350°C;; | |
In neat (no solvent) 5-fold excess of SOCl2 (200°C/3 h);; | |
In thionyl chloride byproducts: NbCl5*SiCl4; |
Conditions | Yield |
---|---|
With pyrographite In neat (no solvent) in stream of COCl2 at 500°C, chlorination of NbOCl3 by passing over heated coal;; | |
With pyrographite In neat (no solvent) in stream of COCl2 at 500°C, chlorination of NbOCl3 by passing over heated coal;; |
Conditions | Yield |
---|---|
In further solvent(s) further solvent: hexachloropropene; refluxing under exclusion of moisture for 4 h, cooling, crystn.;; filtration, washing with cold CCl4, pumping off remaining chlorinated hydrocarbons;; |
Conditions | Yield |
---|---|
In further solvent(s) further solvent: hexachlorobutadiene-(1.3); refluxing in presence of Cl2;; |
Conditions | Yield |
---|---|
In further solvent(s) further solvent: octachloropropane; refluxing;; | |
In further solvent(s) further solvent: octachloropropane; complete chlorination by refluxing;; |
Conditions | Yield |
---|---|
In neat (no solvent) in a sealed tube at 250°C within 2 h;; small yield;; |
Conditions | Yield |
---|---|
In further solvent(s) further solvent: octachlorocyclopentene; refluxing in presence of Cl2;; |
niobium pentachloride
Conditions | Yield |
---|---|
With chlorine In neat (no solvent) | |
With Cl2 In neat (no solvent) |
Conditions | Yield |
---|---|
In neat (no solvent) byproducts: AlOCl; 20 h heating of 248.1 mg Nb2O5 and 1.5 g AlCl3 in molten tube at 270°C;; | |
In neat (no solvent) byproducts: Al2O3, NbOCl3; heating Nb2O5 and AlCl3 in evacuated molten tube at 230, 300 and 400°C;; |
Conditions | Yield |
---|---|
With oxalic acid In water dissolving of NbCl5 in oxalic acid soln.; addn. of a soln. of lead acetate; the pH was adjusted to 9 with aq. NH3;; the ppt. was filtered off, washed and dried at 100°C;; | 100% |
2,6-diisopropylbenzenamine
niobium pentachloride
Conditions | Yield |
---|---|
In dichloromethane inert atmosphere; stirring NbCl5 with excess amine (room temp., 10 h); solvent removal (vac.) drying (vac.); elem. anal.; | 100% |
yttrium(III) chloride
niobium pentachloride
Conditions | Yield |
---|---|
In neat (no solvent) Ar, stoichiometric mixture sealed in a quartz tube, heated at 1023 K for4 d, the heating and cooling ramps were 20 and 10 K*h**-1, respectively; | 99% |
1,2-dimethoxyethane
niobium pentachloride
aniline
cis,mer-Nb(NPh)Cl3(1,2-dimethoxyethane)
Conditions | Yield |
---|---|
With ZnCl2; pyridine In dichloromethane; toluene N2-atmosphere; addn. of 1 equiv. aniline and pyridine (in CH2Cl2) to mixt. of TaCl5 and DME with excess ZnCl2 (-40°C), stirring for 17 h; filtration, concn. (vac.), recrystn. (CH2Cl2/pentane); | 99% |
With pyridine; zinc(II) chloride Inert atmosphere; |
Conditions | Yield |
---|---|
With ZnCl2; pyridine In dichloromethane; toluene N2-atmosphere; addn. of 1 equiv. aniline and pyridine (in CH2Cl2) to mixt. of TaCl5 and DME with excess ZnCl2 (-40°C), stirring for 17 h; filtration, concn. (vac.), recrystn. (CH2Cl2/pentane); | 99% |
With pyridine; zinc(II) chloride Inert atmosphere; |
1,2-dimethoxyethane
niobium pentachloride
naphthalen-2-ylamine
Nb(N-2-naphthyl)Cl3(1,2-dimethoxyethane)
Conditions | Yield |
---|---|
With ZnCl2; pyridine In dichloromethane; toluene N2-atmosphere; addn. of 1 equiv. aniline and pyridine (in CH2Cl2) to mixt. of TaCl5 and DME with excess ZnCl2 (-40°C), stirring for 17 h; filtration, concn. (vac.), recrystn. (CH2Cl2/pentane); elem. anal.; | 99% |
1,2-dimethoxyethane
2-aminoanthracene
niobium pentachloride
Nb(N-2-anthryl)Cl3(1,2-dimethoxyethane)
Conditions | Yield |
---|---|
With ZnCl2; pyridine In dichloromethane; toluene N2-atmosphere; addn. of 1 equiv. aniline and pyridine (in CH2Cl2) to mixt. of TaCl5 and DME with excess ZnCl2 (-40°C), stirring for 17 h; filtration, concn. (vac.), recrystn. (CH2Cl2/pentane); | 99% |
2-methyl-2-butylamine
niobium pentachloride
Conditions | Yield |
---|---|
In diethyl ether; toluene N2-atmosphere; 3 equiv. amine, stirring for 4 h; evapn. (vac.), washing (pentane), drying (vac.); elem. anal.; | 99% |
niobium pentachloride
pentane
benzene
A
4,4'-bis[P-(chlorogold(I))diphenylphosphino]biphenyl
Conditions | Yield |
---|---|
In tetrahydrofuran under N2; soln. of Au complex in THF added to solid NbCl5; stirred at room temp. overnight; volatiles removed in vac.; dissolved in benzene; centrifuged; decanted; concd. in vac.; crystd. from benzene-pentane; elem. anal.; | A 99% B 76% |
diethyl ether
niobium pentachloride
Conditions | Yield |
---|---|
In toluene for 24h; Inert atmosphere; Glovebox; | 99% |
niobium pentachloride
toluene
Conditions | Yield |
---|---|
In toluene mixt. was refluxed for 16 h (N2) and evapd., toluene was added, mixt. was stirred for 20 min; evapd., collected from toluene; elem. anal.; | 98% |
niobium pentachloride
Conditions | Yield |
---|---|
In toluene byproducts: HCl; N2-atmosphere; addn. of NbCl5 to suspension of calix, refluxing (16 h); evapn., addn. of MePh, stirring (20 min), evapn.; elem. anal.; | 98% |
niobium pentachloride
dichlorotris(3,5-di-tert-butylpyrazolato)niobium(V)
Conditions | Yield |
---|---|
In toluene byproducts: KCl; Ar-atmosphere; slight excess of ligand, stirring at room temp. for 16 h; filtration (Celite), removal of volatiles (reduced pressure); elem. anal.; | 98% |
Conditions | Yield |
---|---|
Stage #1: niobium pentachloride With dihydrogen peroxide In water at 8℃; Stage #2: potassium hydroxide In water at 8 - 20℃; | 98% |
Methoxytrimethylsilane
niobium pentachloride
trichlorodimethoxyniobium(V)
Conditions | Yield |
---|---|
In dichloromethane byproducts: trimethylchlorosilane; reaction at -78°C, then was allowed to warm to room temp., concentreting under reduced pressure, hexane was added to give a white crist. solid (all in an inert atmosphere); washing with hexane, dried under vac., elem.anal.; | 97% |
Methoxytrimethylsilane
niobium pentachloride
dichlorotrimethoxyniobium(V)
Conditions | Yield |
---|---|
In dichloromethane byproducts: trimethylchlorosilane; reaction with three or more equiv. trimethylmethoxysilane at -78°C. The mixture was allowed to warm to room temp., concg. under reduced pressure, then hexane was added to give a white cryst. solid (all operations in an inert atmosphere); washing with hexane, dried under vac., elem.anal.; | 96% |
1,2-dimethoxyethane
niobium pentachloride
p-toluidine
[Nb(=NC6H4Me-4)Cl3(dme)]
Conditions | Yield |
---|---|
With ZnCl2; pyridine In dichloromethane byproducts: C5H5NH[ZnCl3]; inert atmosphere; addn. of 2 equiv. ZnCl2 and excess DME to NbCl5, cooling to -30°C, addn. of 1 equiv. of amine, stirring (room temp., 16 h); decantation, filtrtaion, solvent removal (reduced pressure), crystn. (CH2Cl2/hexane, -30°C); elem. anal.; | 96% |
4-trimethylsilyl-N,N-bis(trimethylsilyl)aniline
niobium pentachloride
bis(acetonitrile)trichloro(4-trimethylsilylphenylimido)niobium(V)
Conditions | Yield |
---|---|
In acetonitrile (Ar); addn. of a soln. of ligand in acetonitrile to a soln. of niobium salt in acetonitrile at room temp., stirring for 90 min; evapn., addn. of pentane, drying in vac.; elem. anal.; | 96% |
5,10,15,20-tetraphenyl-21H,23H-porphine
niobium pentachloride
Conditions | Yield |
---|---|
With H2O In benzonitrile Ar-atmosphere; slow addn. of ligand to NbCl5 soln., refluxing (20 h), addn. of H2O; extn. (CHCl3), washing (H2O), drying, chromy. (SiO2 or Al2O3, CHCl3/C6H6=1:2, then CHCl3/MeOH=4:1), recrystn. (C6H6); elem. anal.; | 96% |
niobium pentachloride
1-[dichloro(methyl)silyl]-1-(trimethylsilyl)cyclopentadiene
[NbCl4(η5-C5H4(SiCl2Me))]
Conditions | Yield |
---|---|
In dichloromethane under Ar, Schlenk techniques; soln. of ligand added dropwise to suspn. of NbCl5 (1:1) in CH2Cl2, stirred at room temp. for 16 h; concd., hexane added, crystd. on cooling to -30°C, elem. anal.; | 96% |
titanium
niobium pentachloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) stoich. amts. of Nb powder, Ti foil, CsCl, Nb2O5 and NbCl5 were mixed under Ar, placed in a silica tube, sealed under vac., heated for 4 d at 700°C and cooled to 500°C for 4 d and then to room temp.; | 95% |
Diphenyltrimethylsiloxy-N-trimethylsilylphosphinimid
niobium pentachloride
Conditions | Yield |
---|---|
In dichloromethane byproducts: (CH3)3SiCl; addn. of Me3SiOPPh2NSiMe3 to NbCl5 suspension under N2, -193°C; slowly allowing to warm up to room temp.; stirring, room temp., 12h; pptn.; filtration; washing (n-hexane); drying (vac.); elem. anal.; | 95% |
Hexamethyldisiloxane
niobium pentachloride
acetonitrile
Nb(O)Cl3(CH3CN)2
Conditions | Yield |
---|---|
In acetonitrile byproducts: Me3SiCl; soln. of (Me3Si)2O added dropwise to suspension of NbCl5 at room temp. under N2-atmosphere; mixture stirred for 2 h at room temp.;; filtration, concn., crystn. at -30°C, crystals dried in vacuo, elem. anal.; | 95% |
hexamethyldisilathiane
niobium pentachloride
niobium sulphide trichloride
Conditions | Yield |
---|---|
In dichloromethane Shlenck tube; addn. of soln. of org. compd. in CH2Cl2 to stirred suspn.of NbCl5 in CH2Cl2 (30 min); sepn., washing (CH2Cl2), drying (air); elem. anal.; | 95% |
niobium pentachloride
titanium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) byproducts: Nb3Cl8; Ar atmosphere, TlCl, TiCl3, Nb, NbCl5 in sealed quartz tube at 720 °C for 3 d, heating and cooling rates: 50 °/h; | 95% |
niobium pentachloride
titanium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) byproducts: Nb3Cl8; Ar atmosphere, RbCl, TiCl3, Nb, NbCl5 in sealed quartz tube at 720 °C for 3 d, heating and cooling rates: 50 °/h; | 95% |
niobium pentachloride
titanium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) byproducts: Nb3Cl8; Ar atmosphere, KCl, TiCl3, Nb, NbCl5 in sealed quartz tube at 720 °C for 3 d, heating and cooling rates: 50 °/h; | 95% |
niobium pentachloride
titanium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) byproducts: Nb3Cl8; Ar atmosphere, InCl, TiCl3, Nb, NbCl5 in sealed quartz tube at 720 °C for 3 d, heating and cooling rates: 50 °/h; | 95% |
niobium pentachloride
titanium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) byproducts: Nb3Cl8; Ar atmosphere, CsCl, TiCl3, Nb, NbCl5 in sealed quartz tube at 720 °C for 3 d, heating and cooling rates: 50 °/h; | 95% |
Conditions | Yield |
---|---|
Stage #1: niobium pentachloride With 1-methyl-3,6-bis(trimethylsilyl)-1,4-cyclohexadiene In dichloromethane at 20℃; Stage #2: 2,2'-azopyridine In dichloromethane at 20℃; for 2h; | 95% |
Reported in EPA TSCA Inventory. EPA Genetic Toxicology Program.
The Niobium pentachloride, with the CAS registry number 10026-12-7, is also known as Niobium(V) chloride. It belongs to the product categories of Metal halide; Niobium Salts; Crystal Grade Inorganics; Materials Science; Metal and Ceramic Science; Niobium; Salts. Its EINECS number is 233-059-8. This chemical's molecular formula is Cl5Nb and molecular weight is 270.17. What's more, its systematic name is niobium(+2) cation pentachloride. Its classification code is Mutation data. This chemical should be sealed and stored in a ventilated and dry place. Moreover, it should be protected from light. It hydrolyzes in air, and samples are often contaminated with small amounts of NbOCl3. It is often used as a precursor to other compounds of niobium. This substance is the main precursor to the alkoxides of niobium, which find niche uses in sol-gel processing. It is also the precursor to many other laboratory reagents.
Preparation: Industrially, Niobium pentachloride is obtained by direct chlorination of niobium metal at 300 to 350 °C. In the laboratory, it is often prepared from Nb2O5, the main problem being incomplete reaction to give the oxyhalides. The conversion can be effected with thionyl chloride: It also can be prepared by chlorination of niobium pentoxide in the presence of carbon at 300°C. The products, however, contain small amounts of NbOCl3.
2 Nb + 5 Cl2 → 2 NbCl5
When you are using this chemical, please be cautious about it as the following:
This chemical is harmful by inhalation, in contact with skin and if swallowed. It can cause burns. In case of contact with eyes, you should rinse immediately with plenty of water and seek medical advice. After contact with skin, you should wash immediately with plenty of ... (to be specified by the manufacturer). When using it, you need wear suitable protective clothing, gloves and eye/face protection. After using it, you must ake off immediately all contaminated clothing.
You can still convert the following datas into molecular structure:
(1)SMILES: [Nb+2].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-]
(2)Std. InChI: InChI=1S/5ClH.Nb/h5*1H;/q;;;;;+2/p-5
(3)Std. InChIKey: WYLNVWMMGXVYLE-UHFFFAOYSA-I
The toxicity data is as follows:
Organism | Test Type | Route | Reported Dose (Normalized Dose) | Effect | Source |
---|---|---|---|---|---|
mouse | LD50 | intraperitoneal | 61mg/kg (61mg/kg) | LUNGS, THORAX, OR RESPIRATION: RESPIRATORY DEPRESSION BEHAVIORAL: SOMNOLENCE (GENERAL DEPRESSED ACTIVITY) KIDNEY, URETER, AND BLADDER: URINE VOLUME INCREASED | Toxicology and Applied Pharmacology. Vol. 4, Pg. 385, 1962. |
mouse | LD50 | oral | 829mg/kg (829mg/kg) | Hygiene and Sanitation Vol. 31(7-9), Pg. 328, 1966. | |
rat | LD50 | intraperitoneal | 40mg/kg (40mg/kg) | Environmental Quality and Safety, Supplement. Vol. 1, Pg. 1, 1975. | |
rat | LD50 | oral | 1400mg/kg (1400mg/kg) | Hygiene and Sanitation Vol. 31(7-9), Pg. 328, 1966. |
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