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inquiryOxovanadium,trihydrochloride Application:Oxovanadium,trihydrochloride
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CFTC?PharmaChem?is?a?service?based?company?in?China,?a?pharmachem?division?of?Changzhou?Foreign?Trade?Corp.,supplying?raw?materials,?intermediates,?APIs?and?fine?chemicals?for?the?pharmaceutical?and?specialty?chemical?industries?worldwide. Applicatio
vanadium(V) oxychloride
Conditions | Yield |
---|---|
With chlorine In neat (no solvent) Kinetics; heating in a flow of Cl2 at various temps. and reaction times; 99% yield after 50 min. at 680 °C;; | 99% |
With hydrogenchloride In ethanol; water reaction V2O5 with concentrated HCl in presense a few drops of ethanol on water bath untill pentoxide dissolved giving clear blue soln.; not isolated; | |
In hydrogenchloride at ambient temp.;; | |
With SOCl2 In not given reflux. equimol. quants. V2O5 and SOCl2 for 6-8 h; product distd.; elem. anal.; | |
In hydrogenchloride at ambient temp.;; |
Conditions | Yield |
---|---|
In neat (no solvent) heating (excess SOCl2);; | 74% |
In neat (no solvent) heating equimolar amounts 6 - 8 h at reflux;; | |
In not given at 70 - 75°C;; |
Conditions | Yield |
---|---|
With coal powder In neat (no solvent) distn.;; | 70% |
With pyrographite In neat (no solvent) in 2 h at 180 - 200°C;; | >99 |
With coal powder In neat (no solvent) heating;; |
Conditions | Yield |
---|---|
In neat (no solvent) heating 6 h under N2 at reflux (105 - 130°C);; distn.;; | 65% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
With chlorine In neat (no solvent) Kinetics; heating in a flow of Cl2 at various temps. and reaction times; 64% yield after 50 min. at 300 °C;; | 64% |
Conditions | Yield |
---|---|
In neat (no solvent) distn.;; VOCl3 with 0.1 % Al;; | 60% |
In neat (no solvent) slowly heating at 400°C;; | |
In neat (no solvent) slowly heating at 400°C;; |
Conditions | Yield |
---|---|
With phosphorus pentoxide In neat (no solvent) in 3.5 h at 80 - 90°C;; | 17% |
With P2O5 In neat (no solvent) in 3.5 h at 80 - 90°C;; | 17% |
In diethyl ether passing HCl gas over solvent, V2O5 added;; not isolated;; |
Dichlorodifluoromethane
B
magnesium divanadate (V)
C
carbon dioxide
D
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In neat (no solvent) using a fixed-bed flow reactor system at atmospheric pressure; placing of of Mg3(VO4)2 in quartz reactor; heating at 723 K under 1% CCl2F2/He atmosphere with total flow rate of 30 ml/min for 5 h; monitoring by XRD and GC-TCD; | A n/a B 1% C n/a D n/a |
Conditions | Yield |
---|---|
In neat (no solvent) VOCl3 distd.;; | |
In neat (no solvent) VOCl3 distd.;; |
Conditions | Yield |
---|---|
In neat (no solvent) annealing;; | |
In neat (no solvent) annealing;; |
aluminium trichloride
1-butyl-3-methylimidazolium chloride
A
[VO2Cl2](1-)
B
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In melt in acidic imidazolium/AlCl3 ionic melt at 25°C; not isolated, detd. by (51)V-NMR and IR spectroscopy; |
Conditions | Yield |
---|---|
In not given at ambiente temp.;; | |
In not given at ambiente temp.;; |
Conditions | Yield |
---|---|
In neat (no solvent) |
chlorine
sulfur
A
disulfur dichloride
B
sulfur dichloride
C
vanadiumtetrachloride
D
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In neat (no solvent) heating;; |
vanadium
chlorine
A
vanadiumtetrachloride
B
vanadium(V) oxychloride
Conditions | Yield |
---|---|
With oxygen In neat (no solvent) react. of V powder with gaseous Cl2 in presence of O2 at ambient temp., faster on heating;; VCl4 contaminated with VOCl3 obtained;; | |
With O2 In neat (no solvent) react. of V powder with gaseous Cl2 in presence of O2 at ambient temp., faster on heating;; VCl4 contaminated with VOCl3 obtained;; |
Conditions | Yield |
---|---|
In neat (no solvent) reflux (75°C);; | |
In neat (no solvent) reflux (75°C);; |
Conditions | Yield |
---|---|
With sodium In neat (no solvent) heating (300°C=reflux);; | >99 |
In not given at 250 - 300°C;; |
Conditions | Yield |
---|---|
Kinetics; |
Conditions | Yield |
---|---|
In neat (no solvent) at 300°C;; | |
In neat (no solvent) at 330°C in tube;; | |
In neat (no solvent) react. V2O5 with excess of AlCl3; distn. of VOCl3 and excess of AlCl3 at 300°C; | |
In neat (no solvent) at 330°C in tube;; |
aluminium trichloride
1-ethyl-3-methyl-1H-imidazol-3-ium chloride
A
[VO2Cl2](1-)
B
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In melt in acidic imidazolium/AlCl3 ionic melt at 25°C; not isolated, detd. by (51)V-NMR and IR spectroscopy; |
disulfur dichloride
A
vanadium(III) chloride
B
vanadiumtetrachloride
C
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In not given heating;; |
Conditions | Yield |
---|---|
In neat (no solvent) room temp.;; | |
In neat (no solvent) room temp.;; |
disulfur dichloride
chlorine
A
vanadiumtetrachloride
B
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In neat (no solvent) passing Cl2 stream with S2Cl2 over V2O5 at ambient temp., slow heating;; |
Conditions | Yield |
---|---|
In neat (no solvent) byproducts: COCl2; using a fixed-bed reaction system directly connected to GC-TCD; placing of V2O5 in quartz reactor; injecting of CCl4; heating at 723 K; monitoring by XRD and GC-TCD; |
Conditions | Yield |
---|---|
In neat (no solvent) heating mixture 2 h; cooling down soln.;; TiOCl as pptn.;; | |
In neat (no solvent) | |
In neat (no solvent) |
Conditions | Yield |
---|---|
In neat (no solvent) VOCl3 distd.;; | |
In neat (no solvent) VOCl3 distd.;; | |
In not given at ambiente temp.;; |
Conditions | Yield |
---|---|
In neat (no solvent) reaction at red heat;; |
Conditions | Yield |
---|---|
In neat (no solvent) 280 °C, 1.5 Torr of CCl3F; monitored by gas-phase FT-IR; |
Conditions | Yield |
---|---|
In neat (no solvent) between 200 - 300°C;; |
Conditions | Yield |
---|---|
In neat (no solvent) at 200 - 300°C;; | |
In neat (no solvent) at 200 - 300°C;; |
vanadium(V) oxychloride
trans-1,2-bis[(trimethylsilyl)oxy]cyclohexane
Conditions | Yield |
---|---|
In dichloromethane under Ar, 2 equiv. VOCl3, dropwise addn. of VOCl3 to a stirred soln. of ether in CH2Cl2 in the dark at -78°C, 25°C for 24 h; removal of volatiles by evapn. in vac.; elem. anal.; | 99% |
tris-(trifluoromethyl)methyl hypochlorite
vanadium(V) oxychloride
VO{(CF3)3CO}3
Conditions | Yield |
---|---|
byproducts: (CF3)2CO, CF3Cl, Cl2; stirring at 0°C for 22 h, volatiles removed under vac.; sublimed in vac., elem. anal.; | 99% |
2,6-diisopropylphenyl isocyanate
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In octane N2-atmosphere; refluxing equimolar amts. for 16 h; cooling to 25°C, solvent removal (vac.), solidification on standing at -50°C for 16 h; elem. anal.; | 99% |
In octane byproducts: CO; react. of VOCl3 with ArNCO in refluxing n-octane; elem. anal.; | >99 |
ethyl trimethylsilyl ether
vanadium(V) oxychloride
chloroorthovanadic acid diethyl ester
Conditions | Yield |
---|---|
In dichloromethane byproducts: (CH3)3SiCl; (N2); addn. of 3 equiv. of silane deriv. to CH2Cl2 soln. of vanadium compd. at room temp., stirring for 2 h at room temp.; evapn., elem. anal.; | 99% |
N‑sulfinyl‑2‑methoxyaniline
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In n-heptane for 72h; Schlenk technique; Reflux; | 99% |
spiro[adamantane-2,2'-[2a]homoadamantan]-2'a-one
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In dichloromethane in Ar atmosphere spiro(adamantan-2,2'-homoadamantan-3-one in CH2Cl2 placed in glass tube, frozen to -196 °C, gasphase removed, VOCl3 added, mixt. allowed to anneal to room temp., soln. stirred 1 h; volatiles removed in vac., wshing with n-hexane, residue dissoved in CH2Cl2, cooling to -30 °C, crystn., elem. anal.; | 98.8% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In benzene byproducts: NaCl; anhydrous conditions, addn. of Na-salt to VOCl3 in benzene, refluxed for 12-14 h at 120°C; filtered, evapd., washed with n-hexane, dried in vac. at 40-60°Cfor 3 h, purity checked by TLC; elem. anal.; | 98% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In benzene byproducts: NaCl; anhydrous conditions, addn. of Na-salt to VOCl3 in benzene, refluxed for 12-14 h at 120°C; filtered, evapd., washed with n-hexane, dried in vac. at 40-60°Cfor 3 h, purity checked by TLC; elem. anal.; | 98% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In pentane (Ar); std. Schlenk technique; soln. of V compd. in pentane was added dropwise to stirred soln. of ligand in pentane at -60°C; stirred for2 h while warmed to room temp.; evacuated; washed (pentane); dried (vac.); elem. anal.; | 98% |
Conditions | Yield |
---|---|
In dichloromethane byproducts: (CH3)3SiCl; (N2); addn. of 5 equiv. of silane deriv. to CH2Cl2 soln. of vanadium compd. at room temp., stirring for 16 h at room temp.; evapn., elem. anal.; | 98% |
Conditions | Yield |
---|---|
In hexane a soln. of DME in hexane was added dropwise at room temp. over 30 min toa stirred soln. of VOCl3 in hexane, the mixt. was stirred for 1 h (iner t atm.); ppt. was filtered off, washed with hexane, dried under vac. at room temp.; elem. anal.; | 97% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In benzene byproducts: NaCl; anhydrous conditions, addn. of Na-salt to VOCl3 in benzene, refluxed for 12-14 h at 120°C; filtered, evapd., washed with n-hexane, dried in vac. at 40-60°Cfor 3 h, purity checked by TLC; elem. anal.; | 97% |
ethyl trimethylsilyl ether
vanadium(V) oxychloride
oxovanadium(V) ethoxydichloride
Conditions | Yield |
---|---|
In dichloromethane byproducts: (CH3)3SiCl; (N2); addn. of 2 equiv. of silane deriv. to CH2Cl2 soln. of vanadium compd. at room temp., stirring for 2 h at room temp.; evapn., elem. anal.; | 97% |
Conditions | Yield |
---|---|
In dichloromethane byproducts: (CH3)3SiCl; (N2); addn. of 3 equiv. of silane deriv. to CH2Cl2 soln. of vanadium compd. at room temp., stirring for 2 h at room temp.; evapn., elem. anal.; | 97% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In dichloromethane byproducts: (CH3)3SiCl; (N2); addn. of 10 equiv. of silane deriv. to CH2Cl2 soln. of vanadium compd. at room temp., stirring for 16 h at room temp.; evapn., elem. anal.; | 97% |
Conditions | Yield |
---|---|
In n-heptane for 72h; Reflux; | 97% |
tri-(p-chlorophenyl)-silanol
vanadium(V) oxychloride
tris(tri(p-chlorophenyl)silyl)vanadate
Conditions | Yield |
---|---|
With triethylamine In not given according to H. Pauling et al., Helv. Chim. Acta, 1976, 59, 1233; | 96% |
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In benzene byproducts: NaCl; anhydrous conditions, addn. of Na-salt to VOCl3 in benzene, refluxed for 12-14 h at 120°C; filtered, evapd., washed with n-hexane, dried in vac. at 40-60°Cfor 3 h, purity checked by TLC; elem. anal.; | 96% |
Conditions | Yield |
---|---|
In dichloromethane byproducts: ClSi(CH3)3; (N2); addn. of 3 equiv. of silane deriv. to CH2Cl2 soln. of vanadium compd. at room temp., stirring for 2 h at room temp.; evapn., elem. anal.; | 96% |
vanadium(V) oxychloride
tert-butylamine
B
tert-butylimidovanadium(V) trichloride
Conditions | Yield |
---|---|
In pentane byproducts: H2O; under Ar; slow addn. of amine soln. to dissolved VOCl3 under stirring at -78°C; stirred for 30 min; removing of ice bath; further stirring until reaction mixture was warmed up to 25°C; filtration of (NH3-t-bu-(VOCl3)2O); washed (CH2Cl2 and n-pentane); dried under vac.; solvent removed from mother liquor under vacuo; sublimation of residue (80°C, high vac.); elem. anal.; NMR; IR; | A 95% B 85% |
Triethylgerman
vanadium(V) oxychloride
C
hydrogen
D
triethylchlorogermane
Conditions | Yield |
---|---|
In neat (no solvent) heating reagents;; | A n/a B n/a C n/a D 95% |
In neat (no solvent) heating reagents;; | A n/a B n/a C n/a D 95% |
vanadium(V) oxychloride
{Cl3PNPCl3}(1+)*VOCl4(1-)={Cl3PNPCl3}VOCl4
Conditions | Yield |
---|---|
In dichloromethane moisture excluded, dropwise addn. of CH2Cl2 soln. of VOCl3 to suspension of Cl3PNPCl3Cl in CH2Cl2 (room temp., stirred), clear soln.; concd. in vac., addn. of CCl4, crystn., filtered, washed (CCl4), dried in vac., elem. anal.; | 95% |
Conditions | Yield |
---|---|
With triethylamine In benzene byproducts: triethylamine hydrochloride; soln. of HN(P(C6H5)2NC6H5)2 with triethylamine added drope-wise with stirring to ice-cooled soln. of VOCl3 (under N2) (1:1 molar ratio), broughtto room temp., stirred for 1-2 h; filtered, excess of solvent removed (vac.), dried in vac. for 3 h, purified by dissolving in diethyl ether; elem. anal.; | 95% |
Conditions | Yield |
---|---|
In pentane byproducts: HCl; Schlenk technique, protected from direct sun light; VOCl3 slowly added to soln. of alcohol in n-pentane at 0°C; HCl completely removed by heating at 30°C; crystd. at -30°C overnight; additional portion of crystals obtained by concg. the decanted soln. and storing at -30°C overnight; elem. anal.; | 95% |
t-butyl-N-sulfinylamine
vanadium(V) oxychloride
tert-butylimidovanadium(V) trichloride
Conditions | Yield |
---|---|
In hexane byproducts: SO2; Sonication; (Ar) VOCl3 in hexane at room temp. was added to soiln. t-BuNSO in hexane, refluxed for 2 h; volatiles were removed in vacuo at 20°C, residue was suspnd. in pentane by sonication and kept at -80°C for 24 h, ppt. was decanted, washed with chilled pentane and dried in vacuo; | 95% |
((2,6-diisopropylphenyl)imino)-λ4-sulfanone
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In octane byproducts: SO2; (Ar) VOCl3 and AtNSO in n-octane eas heated at reflux for 3 h; volatiles were removed in vacuo, residue was crystd. from hot hexane by cooling soln. slowly down to -80°C; elem. anal.; | 95% |
(tetrabutylammonium)4H3PW11O39
vanadium(V) oxychloride
Conditions | Yield |
---|---|
In pyridine (Ar); stirring (1 h, 80°C); cooling (room temp.), diethyl ether addn., washing (diethyl ether), drying (vac.); elem. anal.; | 94% |
Conditions | Yield |
---|---|
With triethylamine In benzene byproducts: triethylamine hydrochloride; soln. of (HN(P(C6H5)2NC6H5)2) along with triethylamine added drope-wise with stirring to ice-cooled soln. of VOCl3 (under N2) (2:1 molar ratio),brought to room temp., stirred for 1-2 h; filtered, excess of solvent removed (vac.), dried in vac. for 3 h, purified by dissolving in diethyl ether; elem. anal.; | 94% |
Conditions | Yield |
---|---|
With triethylamine In benzene byproducts: triethylamine hydrochloride; soln. of (HN(P(C6H5)2NSi(CH3)3)2) with triethylamine added drope-wise with stirring to ice-cooled soln. of VOCl3 (under N2) (2:1 molar ratio), brought to room temp., stirred for 1-2 h; filtered, excess of solvent removed (vac.), dried in vac. for 3 h, purified by dissolving in diethyl ether; elem. anal.; | 94% |
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