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inquiryVanadium chloride (VCl3) Application:for chemcial
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inquiryvanadium hexacarbonyl
triphenyllead(IV) chloride
A
(C6H5)3PbV(CO)6
B
vanadium(III) chloride
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under N2 or Ar, exclusion of light, stirred for 24 h at room temp.; filtered (VCl3), partial evapn. in vac. at room temp., cooled to -30°C overnight; elem. anal.; | A 60% B 99% |
Conditions | Yield |
---|---|
In n-heptane byproducts: 1,3,5-trimethylbenzene, H2; under purified Ar atm.; soln. of V(η6-Me3C6H3)2 in heptane was treated with dry HCl; after 2 hs suspn. filtered; solid dried (vac.) at room temp.; elem. anal.; | 98% |
Conditions | Yield |
---|---|
With hydrogen sulfide In benzene treatment with H2S about 20 min at ambiente temp.;; washing pptn. with CCl4 and drying in vacuum at 2 torr and 150°C;; | 98% |
With HI In n-heptane treating a heptane soln. of VCl4 with dry HI; stirring, room temp., 15 h;; filtration; washing solid with heptane; heating, 50°C, 0.05mmHg, 4h; elem. anal.;; | 97% |
In neat (no solvent) decompn. about 50 h;; purifn. in vac.;; | 90% |
vanadium hexacarbonyl
trityl chloride
A
hexaphenylethane
B
vanadium(III) chloride
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under Ar or N2, exclusion of light, stirred for 10 min at room temp.; observed by IR, removal of solvent in vac., extn. (toluene), VCl3 sepd. by filtration, soln. evapd. to dryness in vac. at room temp., washed with n-heptane (C2Ph6); | A 92% B 98% |
vanadium hexacarbonyl
triphenyltin chloride
A
(C6H5)3SnV(CO)6
B
vanadium(III) chloride
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under N2 or Ar, exclusion of light, stirred for 24 h at room temp.; filtered (VCl3), partial evapn. in vac. at room temp., cooled to -30°C overnight; | A 76% B 97% |
vanadium hexacarbonyl
vanadium(III) chloride
Conditions | Yield |
---|---|
With hydrogen chloride In n-heptane byproducts: carbon monoxide, dihydrogen; under Ar or N2, exclusion of light, at -78°C, warmed to -40°C; pptn. filtered off at room temp.; | 96% |
chloro-diphenylphosphine
A
vanadium(III) chloride
B
Tetraphenyldiphosphin
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under Ar or N2, exclusion of light, refluxed for 4 h; filtered hot (VCl3), partial evapn. of solvent, cooled at -78°C (P2Ph4); | A 86% B 91% |
Conditions | Yield |
---|---|
With N2H5Cl In tetrachloromethane heating 10 - 15 h under N2 at reflux;; heating with CS2; pptn. washing with CHCl3 and ether;; | 90% |
With N2H5Cl In tetrachloromethane heating 10 - 15 h under N2 at reflux;; heating with CS2; pptn. washing with CHCl3 and ether;; | 90% |
With toluene In neat (no solvent) heating SOCl2;; |
triethylsilane
vanadiumtetrachloride
A
triethylsilyl chloride
B
vanadium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent) in heating triethylsilane in 5 min;; | A 87% B n/a C n/a |
In neat (no solvent) in heating triethylsilane in 5 min;; | A 87% B n/a C n/a |
vanadium hexacarbonyl
chloro-diphenylphosphine
A
vanadium(III) chloride
B
Tetraphenyldiphosphin
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under Ar or N2, exclusion of light, stirred for 15 h at room temp.; observed by IR, removal of solvent in vac., extn. (toluene), VCl3 sepd. by filtration, soln. evapd. to dryness in vac. at room temp., washed with n-heptane (P2Ph4); | A n/a B 87% |
vanadium hexacarbonyl
benzyl chloride
A
vanadium(III) chloride
B
benzil
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under Ar or N2, exclusion of light, stirred for 12 h at room temp.; observed by IR, removal of solvent in vac., extn. (toluene), VCl3 sepd. by filtration, soln. evapd. to dryness in vac. at room temp., washed with n-heptane (dibenzyl); | A n/a B 81% |
Conditions | Yield |
---|---|
In neat (no solvent) in 24 h in sealed tube at 200°C;; removal of by-products on heating under N2;; | 80% |
In neat (no solvent) in 24 h in sealed tube at 200°C;; distn. SOCl2 in vac.; pptn. washed with CS2 and dried at 80°C in vac.;; | >99 |
vanadium hexacarbonyl
chlorobenzene
A
biphenyl
B
vanadium(III) chloride
Conditions | Yield |
---|---|
In n-heptane byproducts: CO; under Ar or N2, exclusion of light, stirred for 48 h at room temp.; observed by IR, removal of solvent in vac., extn. (toluene), VCl3 sepd. by filtration, soln. evapd. to dryness in vac. at room temp., washed with n-heptane (diphenyl); | A 80% B n/a |
Conditions | Yield |
---|---|
In gas vaporized V reacted with Cl2; | 40% |
In tetrachloromethane slow heating of V (purity 93%) with Cl2 in CCl4 at 100°C;; | |
In neat (no solvent) react. of V powder with gaseous Cl2 on strong heating;; |
Conditions | Yield |
---|---|
In neat (no solvent) heating under exclusion of moisture at reflux; extraction with freshly distd. CCl4 (over P2O5); filtration under N2;; pptn. washed with CCl4 and dried in vacuum;; | |
In melt byproducts: I2; melting of fine V-powder with an excess of ICl, react. starts even on slight warming;; | >99 |
sulfur dioxide
vanadiumtetrachloride
A
thionyl chloride
B
vanadium(III) chloride
Conditions | Yield |
---|---|
byproducts: VOCl3; 2 month; | |
byproducts: VOCl3; 2 month; |
vanadium(V) oxychloride
sulfur
A
sulfur dioxide
B
vanadium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent) at 150°C;; | |
In neat (no solvent) at 150°C;; |
Conditions | Yield |
---|---|
In neat (no solvent) heating 8 h at 400°C in tube; washing with CS2 and heating at 150°C in vacuum;; | >99 |
In neat (no solvent) quant. react. of V-powder with S2Cl2 in a shooting tube at 400°C within 8 h;; solid VCl3 obtained;; | >99 |
Conditions | Yield |
---|---|
In neat (no solvent) heating under back flow, 600°C;; mixture of VCl2 and VCl3 obtained;; |
Conditions | Yield |
---|---|
In neat (no solvent) at 300 - 400°C;; | |
In neat (no solvent) react. of V-powder with sharply dried, streaming HCl-gas at 300 to 400°C;; partially sublimating VCl3 obtained;; |
Conditions | Yield |
---|---|
In neat (no solvent) reaction at 300-400 °C;; |
Conditions | Yield |
---|---|
In neat (no solvent) heating 8 h under reflux;; washing with CS2 and drying in vac. at 120°C;; | |
In neat (no solvent) heating 8 h under reflux;; extraction with CS2;; |
Conditions | Yield |
---|---|
In neat (no solvent) heating under reflux;; | |
In neat (no solvent) | |
In neat (no solvent) |
Conditions | Yield |
---|---|
In neat (no solvent) heating;; | |
In neat (no solvent) heating;; |
Conditions | Yield |
---|---|
In neat (no solvent) 200°C, 24 h; further byproducts: higher chlorides;; | |
In neat (no solvent) 200°C, 24 h; further byproducts: higher chlorides;; |
Conditions | Yield |
---|---|
In not given heating under reflux;; | |
In not given heating under reflux;; |
Conditions | Yield |
---|---|
In neat (no solvent) pure;; | |
heated; washed (CS2); | |
With sulfur In not given at 138°C; equimolar amounts;; |
disulfur dichloride
A
vanadium(III) chloride
B
vanadiumtetrachloride
C
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In not given heating;; |
chlorine
A
disulfur dichloride
B
vanadium(III) chloride
C
vanadiumtetrachloride
Conditions | Yield |
---|---|
In neat (no solvent) at higher temp.;; | |
In neat (no solvent) at higher temp.;; |
Conditions | Yield |
---|---|
With carbon dioxide In neat (no solvent) heating under reflux in CO2 stream at 140 - 150°C;; drying under CO2;; | |
With chlorine In neat (no solvent) distn. of mixt. in Cl2 stream;; washing with ether;; | |
With CO2 In neat (no solvent) heating under reflux in CO2 stream at 140 - 150°C;; drying under CO2;; |
Conditions | Yield |
---|---|
In further solvent(s) byproducts: MeCl; slow heating in neat Ph(Me)P(O)OMe until complete pptn.; particle size and polymerization degree depending on heating rate; | 100% |
Conditions | Yield |
---|---|
In tetrahydrofuran; dichloromethane N2-atmosphere; pptn. on addn. of VCl3 (in THF) to slight excess of ligand (in CH2Cl2); filtration, washing (CH2Cl2); elem. anal.; | 100% |
tetrahydrofuran
vanadium(III) chloride
(THF)2LiCl2VCl2(THF)2 C16H32Cl4LiO4V, monocline
Conditions | Yield |
---|---|
In tetrahydrofuran 1 equiv. of LiCl and VCl3 were mixed in THF, reflux for 10 h, under Ar; crystn. at 20 °C for 3 days, elem. anal.; | 99% |
tetrahydrofuran
vanadium(III) chloride
Vanadium (III) chloride-(tris-tetrahydrofuran)
Conditions | Yield |
---|---|
In tetrahydrofuran heating overnight; hot filtration, crystn. at room temp.; | 99% |
With magnesium boiling for 8 hours in presence of Mg; exclusion of moisture (reaction under N2);; extraction with THF, evaporation and cooling to -10°C; washing with cold THF and recrystallization from THF;; | |
With Mg boiling for 8 hours in presence of Mg; exclusion of moisture (reaction under N2);; extraction with THF, evaporation and cooling to -10°C; washing with cold THF and recrystallization from THF;; | |
In tetrahydrofuran continuous extrn. with THF; |
Conditions | Yield |
---|---|
With urea In quinoline stirred (205-210°C); elem.anal.; | 98% |
Conditions | Yield |
---|---|
In hydrogenchloride extraction from 0.5n-HCl with 6M-NH4SCN with methyl isobutyl ketone;; | 96% |
In water soln. of V(SCN)3 obtained;; |
vanadium(III) chloride
VCl2(C4OH8)2
Conditions | Yield |
---|---|
With tetrahydrofuran; zinc In tetrahydrofuran a complexes was extracted twice in Soxhlet extractor for 3-4 days onto zinc, Ar atm.; filtration, washing a ppt. with THF, drying in vac.; elem. anal.; | 96% |
vanadium(III) chloride
tripotassium 1,4,7-tris-(5-t-butyl-2-hydroxylatobenzyl)-1,4,7-triazacyclononane
V((C2H4)3(NCH2C6H3(O)C(CH3)3)3)
Conditions | Yield |
---|---|
With triethyl amine In acetonitrile refluxing of VCl3 in MeCN (Ar atmosphere), addn. of org. compds.; pptn. on addn. of H2O; elem. anal.; | 96% |
vanadium(III) chloride
Conditions | Yield |
---|---|
With H2O; O2 In further solvent(s) byproducts: HCl; refluxed in water-free 1,2,4-trichlorobenzene for 2 h (under Ar); 1,2,4-trichlorobenzene removed in vac.; residue dissolved in dichloromethane; filtered; chromd. (Al2O3); solvent removed from single fraction obtained; dried in vac.; | 96% |
Conditions | Yield |
---|---|
In neat (no solvent) (Ar); to VCl3 was added CF3SO3H and refluxed for 3 h, green solid formed; solid sepd. and dried in vac.; elem. anal.; | 95% |
With water byproducts: HCl; reaction of VCl3 with CF3SO3H in an O2-free glove box; treatment of the reaction mixt. with H2O distilled onto the mixt., removal of formed HCl and final vacuum drying, elem. anal.; | |
In trifluoroacetic acid mixt. of VCl3 in neat triflic acid heated at reflux under Ar; cooled to room temp., ppt. collected; |
Conditions | Yield |
---|---|
With magnesium hydride In tetrahydrofuran byproducts: H2; (argon); grinding VCl3 and MgH2 in a mill, addn. of -70°C cold THF, then slow addn. of TiCl4, heating to reflux temp. under further grinding (5 h); washing (THF), drying (vac.); | 94.4% |
With sodium In neat (no solvent) reaction by redn. of solid VCl3 with Na in presence of CaCl2 in a bomb (vacuum or inert gas atmosphere), heating at light red heat for a period up to 3 hours;; 95% metallic V;; | 93% |
With hydrogen In neat (no solvent) reaction by redn. of VCl3 with H2 in a stepwise procedure;; metallic V obtained;; | 90% |
Conditions | Yield |
---|---|
With aq. NaOH In ethanol; water pH 2.5; heating (60-80°C, 10 min); elem. anal.; | 92.7% |
vanadium(III) chloride
Conditions | Yield |
---|---|
With H2 In neat (no solvent) at 750°C;; 99.6% VCl2 unpured with 0.25% VCl3 and <0.1% Fe;; | 92% |
With tin byproducts: SnCl2; reaction at 16.2 and 58°C;; | |
With hydrogen In neat (no solvent) reaction started at 480°C;; |
Conditions | Yield |
---|---|
With sodium amalgam In tetrahydrofuran under oxygen-free nitrogen or argon or vac.; 2,2'-bpyridin was added toa suspn. of VCl3 and sodium amalgam in THF; after stirring for 24 h at room temp. and filtering, the soln. was reduced under vac.; diethyletherwas slowly added; ppt. was collected, washed with petroleum (b.p.40-60°C) and recrystd. from THF-diethylether; | 92% |
vanadium(III) chloride
N,N',N''-trimethyl-1,4,7-triazacyclononane
trichloro(1,4,7-trimethyl-1,4,7-triazacyclononane)vanadium(III)
Conditions | Yield |
---|---|
In acetonitrile heating of a soln. of VCl3 in dry acetonitrile to reflux for 10 min; precipitation on cooling of the soln.; addn. of a CH3CN soln. of the organic compound to the mixture; heating to reflux for 30 min; precipitation;; | 92% |
4,4,5,5-tetramethyl-2-thioxo-2λ5-[1,3,2]dioxaphospholane-2-thiol
vanadium(III) chloride
V[S2PO(C(CH3)2)2O]3
Conditions | Yield |
---|---|
In benzene byproducts: HCl; exclusion of moisture; soln. of alkylene dithiophosphoric acid in C6H6 added dropwise with constant stirring to VCl3 in C6H6, molar ratio 3:1, refluxed for ca. 6 h; evapd. in vac., washed with n-hexane (several times), dried in vac.; elem. anal.; | 92% |
N,N,N,N,N,N-hexamethylphosphoric triamide
vanadium(III) chloride
VCl3(((CH3)2N)3PO)3
Conditions | Yield |
---|---|
In tetrahydrofuran (N2), VCl3 extracted into dry THF, organic compound added; collected, washed with n-hexane, pumped in vac. at room temp. for several hours; elem. anal.; | 91% |
2,2':6,2''-terpyridine
vanadium(III) chloride
V(III)(2,2':6',2''-terpyridine)Cl3
Conditions | Yield |
---|---|
In acetonitrile (Ar); to soln. of VCl3 was added ligand, soln. stirred for 4 h, color then had charged from purple to brown; brown ppt. was sepd., washed with diethylether and dried in vac.; elem. anal.; | 91% |
vanadium(III) chloride
1,4,7-tri(iso-propyl)-1,4,7-triazacyclononane
{V(C15H33N3)Cl3}
Conditions | Yield |
---|---|
In acetonitrile refluxing a suspension of VCl3 in dry CH3CN under argon; addn. of C15H33N3 in CH3CN; refluxing for 0.5 h;; pptn. on cooling to 20°C; elem. anal.;; | 91% |
vanadium(III) chloride
1,4,7-triazacyclononane
(1,4,7-triazacyclononane)VCl3
Conditions | Yield |
---|---|
In acetonitrile Ar-atmosphere; refluxing VCl3 to dissoln., addn. of ligand at 40°C, refluxing for 1 h; pptn. on cooling to 10°C, collection (filtration); | 91% |
In N,N-dimethyl-formamide addn. of ligand to soln. of VCl3, refluxing (1 h); pptn. on cooling (room temp.), filtration, washing (Et2O), drying (air); elem. anal.; | 23% |
niobium pentachloride
vanadium(III) chloride
Conditions | Yield |
---|---|
In neat (no solvent) (Ar); sealed in a silica tube under vac., heated at 740°C for 1 wk followed by slow cooling to 550°C in 48 h; radiative cooling to room temp.; | 90% |
vanadium(III) chloride
1,3,5-trimethyl-benzene
bis(mesitylene)vanadium(0)
Conditions | Yield |
---|---|
With Al; AlCl3 In 1,3,5-trimethyl-benzene heating suspension of VCl3, Al powder and AlCl3 in mesitylene at 120-130°C for 2 h, under purified Ar atmosphere; addn. of heptane and THF at 20-25°C under vigorous stirring; mechanism discussed;; filtration after 3 h; removal of volatiles in vac. at 50°C; treating residue with heptane; filtration; washing carefully with heptane; cooling to -78°C;; | 90% |
With Al; AlCl3 In 1,3,5-trimethyl-benzene heating suspension of VCl3, Al powder and AlCl3 in mesitylene at 120-130°C for 2 h, under purified Ar atmosphere; addn. of heptane and DMF at 20-25°C under vigorous stirring; mechanism discussed;; filtration after 3 h; removal of volatiles in vac. at 50°C; treating residue with heptane; filtration; washing carefully with heptane; cooling to -78°C;; | 70% |
With AlBr3; Al In 1,3,5-trimethyl-benzene sublimation, recrystn. from pentane; | 14% |
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