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inquiryVanadium, bis(h6-benzene)-Appearance:Off white to slight yellow solid Storage:Store in dry and cool condition Package:25kg or according to cutomer's demand Application:Chemical research/Pharmaceutical intermediates Transportation:By Sea,by Air,By cou
CAS: [12129-72-5] Molecular Weight: 207.16 Color and Form: black crystals Solubility in Water: Insoluble
potassium{bis(η6-benzene)vanadium(-1)}
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With carbon monoxide In tetrahydrofuran reaction time: 15 minutes; product in mother liquor; by-product is THF-insoluble; highly pyrophoric brownish powder; | 95% |
With carbon dioxide In tetrahydrofuran byproducts: potassium hydrogencarbonate, potassium formiate, potassium oxalate; room temperature; atmospheric pressure, CO2 reacted instantly; filtration; precipitate dried in vacuo (by-products); vacuum evaporation of mother liquor; | 95% |
With carbon dioxide In tetrahydrofuran byproducts: potassium hydrogencarbonate, potassium oxalate, potassium carbonate; sealed ampoule; THF solution saturated with CO2; composition of by-products is substantially different; |
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With carbon dioxide In tetrahydrofuran reaction of V-complex with CO2-saturated THF in a stream of CO2; filtn., washing the THF-insoluble product with THF, drying in vacuo, evapn. of mother liquor yields V-compd.; | 83% |
Conditions | Yield |
---|---|
With AlCl3; THF; benzene In tetrahydrofuran; benzene a mixt. of VCl3, Al and AlCl3 in benzene is refluxed for 15 h under Ar, filtration, slow addn. of the lower layer to THF at room temp. during 2 h, the soln. is stirred 15 h at room temp.; cooled to -30°C overnight, filtration, washed (THF), briefly dried (vac.), the V(0)-compd. is isolated from the concd. soln. at -78°C; | A 60% B 75% |
Conditions | Yield |
---|---|
With aluminium trichloride; sodium dithionite; aluminium In benzene mixt. of VCl3, Al powder, AlCl3, and C6H6 is boiled, dild. with C6H6, and slowly poured in a well cooled 30% KOH soln. containing Na2S2O4; recryst. from diethyl ether; | 27% |
With AlCl3; Al; Na2S2O4 In benzene mixt. of VCl3, Al powder, AlCl3, and C6H6 is boiled, dild. with C6H6, and slowly poured in a well cooled 30% KOH soln. containing Na2S2O4; recryst. from diethyl ether; | 27% |
With aluminium trichloride; sodium dithionite; aluminium In benzene C6H6-VCl3-AlCl3-Al mixt. heated in a sealed tube at 150°C; hydrolysis with aq. KOH soln. containing Na2S2O4; | |
With aluminium trichloride; sodium dithionite; aluminium In benzene C6H6-VCl3-AlCl3-Al mixt. heated in a sealed tube at 150°C; hydrolysis with aq. KOH soln. containing Na2S2O4; |
tetrahydrofuran
benzene
A
(C5H5)DyI2(THF)3
B
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
In benzene Schlenk techniques; V compd. (1.1 mmol) in benzene mixed with iodide (4.54 mmol), stirred at 80°C for 10 h; filtered, solvent evapd., extd. (hexane), evapd., sublimed (100-110°C, 0.1 Torr); residue after extn. recrystd. (THF); | A 5% B 24% |
Conditions | Yield |
---|---|
With dysprosium(II) iodide In benzene under conditions precluding exposure to atm.; soln. of vanadocene in benzene added to powder DyI2 at about 20°C; mixt. heated with stirring to 85°C for 10 h; soln. sepd. from ppt.; benzene removed (vac.); residue extd. (hexane); solvent removed at room temp.; residue heated in vac. by gradually raising the temp. to 110°C; mixt. of crystals sepd. by repeated sublimation (vanadocene sublimed at 50-60...; | 15% |
tetrahydrofuran
benzene
A
(C5H5)NdI2(THF)3
B
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
In benzene Schlenk techniques; V compd. (1.93 mmol) in benzene mixed with iodide (8.69 mmol), stirred at 80°C for 10 h; filtered, solvent evapd., extd. (hexane), evapd., sublimed (100-110°C, 0.1 Torr); residue after extn. recrystd. (THF); | A n/a B 10% |
A
(C6H5C6H5)2V
B
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With MgCl2 evapn. to dryness; sublimation at (1E-3)-(1E-4) torr, 90-120°C; recrystn. from hexane; |
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With MgCl2 In diethyl ether treatment with anhydrous MgCl2 in ether, followed by hydrolysis; | |
With MgCl2 In diethyl ether treatment with anhydrous MgCl2 in ether, followed by hydrolysis; |
Conditions | Yield |
---|---|
With C6H6 In solid matrix V atoms deposited with benzene matrix at 12 K; not isolated, detected by UV, ESR; | |
With C6H6 In solid matrix V atoms deposited with benzene/Ar matrix at 12 K; not isolated, detected by UV, ESR; |
vanadium
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With C6H6 In neat (no solvent, gas phase) low-temp. cocondensation of atomic metal and ligand-vapor; recondensation under vacuum; | |
With benzene In neat (no solvent) cocondensation (12 K, argon); not separated; |
vanadium
benzene
A
V2(η6-benzene)2(μ2-η6:η6-benzene)
D
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
In gaseous matrix V vapour produced via laser vaporization carried by He into a flow tube reactor where C6H6 vapour injected; not isolated, detected by MS; |
Conditions | Yield |
---|---|
With sodium hydroxide; aluminium trichloride; aluminium In benzene reaction in abs. benzene at boiling temp.; removal of C6H6, layering with petroleum ether, hydrolysis with 1N NaOH; (C6H6)2V obtained from the petroleum ether layer is sublimated in high vacuum; | 13-25 |
With (C2H5)3Al or (C2H5MgBr In benzene reaction under Ar; for VCl4, vanadyl acetonate may be used; | 20-30 |
With aluminium trichloride; sodium dithionite; aluminium In benzene AlCl3 in excess; reaction at boiling temp.; removal of C6H6, layering with petroleum ether, hydrolysis with 30% KOH contg. Na2S2O4 at temps. below -3°C; sublimation in high vacuum; | 36-46 |
Conditions | Yield |
---|---|
With phenylmagnesium bromide In tetrahydrofuran addn. of the V complex to PhMgBr in THF at -15°C; addn. of oxygen-free H2O; filtration; evapn.; (C6H5)2 sublimated off; extn. of the residue with hexane/ether (3:1); from the mixt. of (C6H6)2V and (C6H5C6H5)2V, (C6H6)2V is isolated by recrystn. from ether at -20°C; | |
With C6H5MgBr In tetrahydrofuran addn. of the V complex to PhMgBr in THF at -15°C; addn. of oxygen-free H2O; filtration; evapn.; (C6H5)2 sublimated off; extn. of the residue with hexane/ether (3:1); from the mixt. of (C6H6)2V and (C6H5C6H5)2V, (C6H6)2V is isolated by recrystn. from ether at -20°C; |
monobenzene vanadium
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With C6H6 In solid matrix warmed benzene/Ar matrix with V complex from 12 K to 40 K; not isolated, detected by UV, ESR; |
vanadium trichloride tristetrahydrofuran
A
(C6H5C6H5)2V
B
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With phenylmagnesium bromide In tetrahydrofuran addn. of the V complex to PhMgBr in THF at -15°C; addn. of oxygen-free H2O; filtration; evapn.; (C6H5)2 sublimated off; extn. of the residue with hexane/ether (3:1); from the mixt. of (C6H6)2V and (C6H5C6H5)2V, (C6H6)2V is isolated by recrystn. from ether at -20°C; | |
With C6H5MgBr In tetrahydrofuran addn. of the V complex to PhMgBr in THF at -15°C; addn. of oxygen-free H2O; filtration; evapn.; (C6H5)2 sublimated off; extn. of the residue with hexane/ether (3:1); from the mixt. of (C6H6)2V and (C6H5C6H5)2V, (C6H6)2V is isolated by recrystn. from ether at -20°C; |
divanadium
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With benzene In neat (no solvent) cocondensation (12 K, argon); not separated; |
n-butyllithium
bis(η(6)-benzene)vanadium
N,N,N,N,-tetramethylethylenediamine
Conditions | Yield |
---|---|
In n-heptane under Ar atm. soln. V complex in heptane was treated with tmeda and BuLiat room temp. and heated to 80°C for 16 h; ppt. was filtered, washed with pentane, and dried in vacuo; elem. anal.; | 85% |
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With potassium In tetrahydrofuran addn. of THF and potassium sand to V-complex, stirring for 4 h under protective gas; filtn. of unreacted K, analysing of K, concn. of mother liquor in vacuo, addn. of Et2O, standing at -40°C overnight, filtn.; | 68.5% |
bis(η(6)-benzene)vanadium
[Ga(C(Si(CH3)3)2(Si(CH3)2N(CH3)2))Cl2]
benzene
Conditions | Yield |
---|---|
With n-BuLi; TMEDA In diethyl ether standard Schlenk techniques; n-BuLi in hexanes added dropwise to V(C6H6)2 and TMEDA in cyclohexane under reflux; 1 h; cooled to 0°C; solid dried in vac.; slurry in Et2O added to Ga compd. in Et2O (-20°C); stirred (ambient temp., 16 h); crystd. from benzene; elem. anal.; | 58% |
Conditions | Yield |
---|---|
With n-BuLi; Me2NCH2CH2NMe2 In hexane; cyclohexane refluxing (1 h), Me3GeCl soln. (cyclohexane) addn. (0°C), stirring (12 h); filtering, evapn. (reduced pressure), petroleum ether / Et2O (3 : 1) addn., chromy. (SiO2, petroleum ether / Et2O, toluene), fractionally subliming (70 > T > 25°C); elem. anal.; | 56% |
bis(η(6)-benzene)vanadium
[Al(C(Si(CH3)3)2(Si(CH3)2N(CH3)2))Cl2]
benzene
Conditions | Yield |
---|---|
With n-BuLi; TMEDA In diethyl ether standard Schlenk techniques; n-BuLi in hexanes added dropwise to V(C6H6)2 and TMEDA in cyclohexane under reflux; 1 h; cooled to 0°C; solid dried in vac.; slurry in Et2O added to Al compd. in Et2O (-20°C); stirred (ambient temp., 16 h); crystd. from benzene; elem. anal.; | 54% |
bis(η(6)-benzene)vanadium
water
oxygen
ethenetetracarbonitrile
Conditions | Yield |
---|---|
In water; acetonitrile bis(benzene)vanadium reacted with tetracyanoehtylene in CH3CN at room temp. (vac.), stood in air for 1 h; washed (benzene), heated (vac.), elem. anal.; | 50% |
Conditions | Yield |
---|---|
With n-BuLi In diethyl ether; hexane; cyclohexane N2 atm.; refluxing (1.5 h), cooling, decantation, washing (petrolether),stirring (overnight); filtn., extraction (toluene), layering (petrolether), cooling (3 d, -25°C); elem. anal.; | 47% |
1,1-dimethylsilacyclobutane
bis(η(6)-benzene)vanadium
(V(C6H5)2)Si(CH2)3
Conditions | Yield |
---|---|
With BuLi; tetramethylethylenediamine In petroleum ether treatment of V-complex (in cyclohexane) with BuLi (in hexane) and TMEDAat 85°C for 1 h, cooling to room temp., decantation, addn. of petroleum ether, slow addn. of silane (over 2 h, -15°C), stirring (30°C, 12 h); filtration over SiO2, crystn. (-25°C); elem. anal.; | 46% |
bis(η(6)-benzene)vanadium
trimethyltin(IV)chloride
(Me3Sn-η6-C6H5)2V
Conditions | Yield |
---|---|
With n-BuLi; TMEDA In diethyl ether; hexane; cyclohexane N2 atm.; refluxing (1.5 h), cooling, decantation, washing (petrolether),stirring (overnight); filtn., extraction (toluene), layering (petrolether), cooling (3 d, -25°C); elem. anal.; | 44% |
bis(η(6)-benzene)vanadium
tris(pentafluorophenyl)borate
water
toluene
malononitrile
Conditions | Yield |
---|---|
In toluene byproducts: H2, C6H6; (Ar); B(C6F5)3 in toluene added to a soln. of CH2(CN)2, stirred for 1 h,a soln. of V complex added; crystd. for 2-3 d at room temp.; elem. anal.; | A n/a B 40% |
bis(η(6)-benzene)vanadium
{bis(η6-phenyl)(Cl)(4-n-propylphenyl)silane}vanadium
Conditions | Yield |
---|---|
With n-C4H9Li; TMEDA In cyclohexane (N2); the vanadium-compd. is metalated at 85°C during 2 h with n-BuLi and TMEDA, the mixture is cooled to ambient temp., decanted, petroleum ether is added, at -15°C the silane is added dropwise during 1 h; the mixture is kept at room temp. for 12 h and filtered over silylated silica gel, cooling to -20°C, greenish brown material is recrystd. from toluene, elem. anal.; | 38% |
bis(η(6)-benzene)vanadium
toluene
Conditions | Yield |
---|---|
In toluene byproducts: H2; (Ar); a soln. of V complex quickly added to a soln. of B compd.; crystd.; elem. anal.; | 38% |
bis(η(6)-benzene)vanadium
dimesitylfluoroborane
bis[η(6)-dimesitylborylbenzene]vanadium
Conditions | Yield |
---|---|
With n-butyllithium; N,N,N,N,-tetramethylethylenediamine In diethyl ether; cyclohexane addn. of Me2NCH2CH2NMe2 to the V complex in cyclohexane, reflux (1 h), addn. of n-BuLi in cyclohexane, further reflux (1.5 h), cooling to r.t., decant., washing, addn. of Et2O, cooling to -20°C, addn. of FB(mes)2 over 30 min, stirring (12 h); filtration, evapn., recrystn. (petroleum ether); elem. anal.; | 35.6% |
bis(η(6)-benzene)vanadium
N,N,N,N,-tetramethylethylenediamine
diphenylsilyl dichloride
(1-6:1'-6'-η-tetraphenylsilane)vanadium
Conditions | Yield |
---|---|
With n-butyllithium In cyclohexane (N2); dry solvents; addn. of n-BuLi to refluxing soln. of V-compd./TMEDA in C6H12, cooling to room temp., stirring (12 h), removal C6H12, addn. of petroleum ether, cooling to -15°C, addn. of Cl2SiPh2 over 1 h, stirring and warming (20 h); filtration, extn. (hot toluene), crystn. by slow cooling to -25°C; elem. anal.; | 35% |
bis(η(6)-benzene)vanadium
dichlorodimethylgermanium
((CH3)2Ge(C6H5)2)V
Conditions | Yield |
---|---|
With n-BuLi; Me2NCH2CH2NMe2 In hexane; cyclohexane refluxing (1.5 h), decanting (room temp.), washing (petroleum ether), petroleum ether addn., Me2GeCl2 soln. (petroleum ether) addn. (-20°C), stirring (room temp., 2 h); filtering, pptn. (-25°C); elem. anal.; | 34% |
bis(η(6)-benzene)vanadium
Phenyltrichlorosilane
{bis(η6-phenyl)(Cl)phenylsilane}vanadium
Conditions | Yield |
---|---|
With n-C4H9Li; TMEDA In cyclohexane (N2); the vanadium-compd. is metalated at 85°C during 2 h with n-BuLi and TMEDA, the mixture is cooled to ambient temp., decanted, petroleum ether is added, at -15°C the silane is added dropwise during 1 h; the mixture is kept at room temp. for 12 h and filtered over silylated silica gel, cooling to -20°C, greenish brown material is recrystd. from toluene, elem. anal.; | 33% |
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
In benzene byproducts: H2; (Ar); a soln. of V complex quickly added to a soln. of B compd.; crystd. for 3-4 d; elem. anal.; | 33% |
bis(η(6)-benzene)vanadium
chlorodimethylphosphine
A
(η6-benzene)(dimethylphosphano-η6-benzene)vanadium
B
bis(dimethylphosphano-η6-benzene)vanadium
Conditions | Yield |
---|---|
With n-BuLi; N,N,N',N'-tetramethylethylenediamine In hexane; cyclohexane (Ar); Schlenk technique; V complex/C6H12 reacted with BuLi/hexane and amine at 80°C for 2 h; ccoled to room temp.; P compd./C6H12 added with stirring during 30 min; reacted for 24 h; volatiles removed (vac.); dissolved in pentane; chromd. (silica gel, pentane); elem. anal.; | A 32% B 32% |
bis(η(6)-benzene)vanadium
dichlorodiphenylgermane
((C6H5)2Ge(C6H5)2)V
Conditions | Yield |
---|---|
With n-BuLi; Me2NCH2CH2NMe2 In hexane; cyclohexane refluxing (1.5 h), decanting (room temp.), washing (petroleum ether), petroleum ether addn., Ph2GeCl2 soln. (petroleum ether) addn. (-20°C), stirring (room temp., 2 h); filtering, washing (petroleum ether), toluene addn., crystn. on concg. (vac., -10°C); elem. anal.; | 29% |
Conditions | Yield |
---|---|
With n-BuLi; Me2NCH2CH2NMe2 In diethyl ether; hexane; cyclohexane refluxing (1.5 h), decanting (room temp.), washing (petroleum ether), Et2O and Ph3GeCl soln. (Et2O) addn., stirring (overnight); filtering, extg. (boiling toluene), crystn. on petroleum ether addn. (-25°C, 24 h); elem. anal.; | 21% |
1,1,3,3-tetramethyl-1,3-disiletane
bis(η(6)-benzene)vanadium
(V(C6H5)2)2Si2(CH2)2
Conditions | Yield |
---|---|
With BuLi; tetramethylethylenediamine In petroleum ether treatment of V-complex (in cyclohexane) with BuLi (in hexane) and TMEDAat 85°C for 1 h, cooling to room temp., decantation, addn. of petroleum ether, slow addn. of silane (over 3 h, -15°C), stirring (room temp., 12 h); solvent removal (vac.), dissoln. in PhMe, filtration over SiO2, concn.,cooling (crystn.); elem. anal.; | 15% |
bis(η(6)-benzene)vanadium
Conditions | Yield |
---|---|
With n-BuLi; TMEDA In diethyl ether; hexane; cyclohexane N2-atmosphere; addn. of BuLi (hexane) to soln. of V-complex and TMEDA (C6H12), refluxing for 1.5 h, cooling, decantation, washing (petroleum ether), addn. of Et2O, addn. of Zr-complex at -40°C, stirring for 2 h at room temp.; collection (filtration), extn. (boiling MePh), crystn. on cooling to -25°C; elem. anal.; | 14% |
bis(η(6)-benzene)vanadium
μ-(η6:η6-Biphenyl)-bis[(η6-benzol)vanadium(0)]
Conditions | Yield |
---|---|
With n-butyllithium; water In methyl cyclohexane Ph2V soln. added in N2 atm. to n-BuLi in presence of tetramethylene diamine at 90°C for 4 h, cooled to -10°C for 7 h, then room temp. for 9 h, hydrolized for 1 h; dissolved in toluene, chromy., sublimed at 180-210°C, crystd. from toluene, petroleum ether; | 13% |
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