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Tungstenchloride (WCl4), (T-4)- (9CI) Storage:keep in dry and cool condition Package:25kg or according to cutomer's demand Application:Chemical research/pharma intermediate Transportation:By Sea,by Air,By courier like DHL or Fedx. Port:Shanghai/Shenz
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Tungstenchloride (WCl4), (T-4)- (9CI)Appearance:Off white to slight yellow solid Storage:Stored in shaded, cool and dry places Package:1L 5L 10L 25L bottle Application:pharma intermediate Transportation:Handle with cares to avoid damaging the package
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inquiryConditions | Yield |
---|---|
strong HCl; | 100% |
strong HCl; | 100% |
tungsten(VI) chloride
tungsten(IV) chloride
Conditions | Yield |
---|---|
With Sn In 1,2-dichloro-ethane byproducts: SnCl4; absence of air and moisture; stirring with Sn-powder at room temp. for 17 h, then at 80-90°C for 2 d; centrifugation, washing (CH2Cl2), drying (vac., room temp.); elem. anal.; | 98% |
With Sb In neat (no solvent) byproducts: SbCl3, WOCl4, WCl5; absence of air and moisture; sealed evacuated glass tube, 75-80°C(12 h), 105°C (12 h), 130°C (12 h); distn. off of byproducts (130°C, 1d; then 160°C, 1 d; then215°C, 1 d); elem. anal.; | 97% |
With red phosphorus In neat (no solvent) byproducts: PCl3, WOCl4, WCl5; absence of air and moisture; sealed evacuated glass tube, slow heating to 200°C (over 12 h), then to 300°C (over further 12 h); sublimation off of byproducts (230-240°C, 1 d, trap at liquid N2-temp.; further byproduct: POCl3); elem. anal.; | 94% |
Conditions | Yield |
---|---|
In neat (no solvent) byproducts: PCl3; WCl6 and red P (1:1.34) mixed (Ar), sealed (vac.) in silica tube, heatedat 500°C for 24 h; sublimated, XRD; | A 95% B 5% |
Conditions | Yield |
---|---|
In 1,2-dichloro-ethane at 20℃; for 17h; | 93% |
hydrogenchloride
aluminium trichloride
tungsten(VI) chloride
aluminium
sodium chloride
B
tungsten(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) other Radiation; sealing WCl6, Al, AlCl3 and NaCl and Mo into SiO2 ampoule (1E-2 Torr N2), microwave oven (200 W, 60 min, cooling to room temp., further irradiation at 200 W for 60 min), opening, dissoln. in hot concd. HCl; filtration (Celite), crystn. on cooling, washing (cold. concd. HCl, Et2O), drying (overnight); elem. anal.; | A 48% B n/a |
tungsten(VI) chloride
tungsten
A
tungsten(VI) oxychloride
C
tungsten(IV) chloride
Conditions | Yield |
---|---|
reaction of WCl6 with W at 270-750°C for 14 h under a vacuum; removal of WCl4 and WOCl4 byproducts by sublimation, intermediate (H3O)2W6Cl14*6H2O obtained after recrystn. from boiling HCl and cooling to -10°C; intermediate heated at 450°C under a dynamic vacuum; | A n/a B 25% C n/a |
tetrachloromethane
B
tungsten(VI) chloride
C
tungsten(IV) chloride
D
tungsten dioxydichloride
Conditions | Yield |
---|---|
In neat (no solvent) reaction on heating WO2 with CCl4 to 250°C in a closed tube for 8h;; | |
In neat (no solvent) reaction on heating WO2 with CCl4 to 250°C in a closed tube for 8h;; |
Conditions | Yield |
---|---|
In gas Kinetics; Irradiation (UV/VIS); stationary photolysis in a glass cell; flash photolysis in a sealed quartz cell; vac. distn.; |
hydrogen
tungsten(VI) chloride
A
tungsten(V) chloride
B
chlorine
C
tungsten(IV) chloride
Conditions | Yield |
---|---|
In gas Kinetics; byproducts: HCl; Irradiation (UV/VIS); flash photolysis in a sealed quartz cell at 388 K and 403 K; stationaryphotolysis in a sealed glass cell at 140°C; vac. distn.; |
Conditions | Yield |
---|---|
In neat (no solvent) sealed ampoule (270-280 °C, 15 h), molar ratio WCl6:Al = 1:1.5; | |
In neat (no solvent, solid phase) reaction in glass ampules at 400°C; |
tungsten
tungsten(IV) chloride
Conditions | Yield |
---|---|
With Cl2 Kinetics; pulsed chlorine molecular beam reaction with W (300-1350°C, modulated beam-mass spectrometric equipment, base pressure 1E-9 Torr); MS; WCl4 is main product up to ca. 1000°C; | |
With Cl Kinetics; pulsed atomic chlorine beam (generated by RF plasma discharge) reaction with W (300-1350°C, modulated beam-mass spectrometric equipment, base pressure 1E-9 Torr); MS; WCl4 is main product up to ca. 1000°C; |
tungsten(VI) chloride
B
tungsten(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) equimolar amts.; sealed evacuated ampoule, 200-250°C (2 h; condensation of WOCl4 in cold part), then heating to 360°C; elem. anal.; | |
stoich. mixt. heating (evac. sealed two-section ampoule, 200-250°C for 2 h, WOCl4 crystn. in cold part of ampoule), temp. raising to 360°C; thermogravimetric and differential thermal anal.; |
Conditions | Yield |
---|---|
heating at 280°C in a closed tube by melting; | |
heating at 280°C in a closed tube by melting; |
tungsten(VI) chloride
A
tungsten(V) chloride
B
tungsten(IV) chloride
Conditions | Yield |
---|---|
With hydrogen redn. above 350°C; heating in H2 or CO2-stream, distn.; | |
With hydrogen redn. above 350°C; heating in H2 or CO2-stream, distn.; |
Conditions | Yield |
---|---|
In chlorobenzene byproducts: CO; under N2 solvent was added to mixt. of educts; stirring at reflux ca 12h; filtration, washing with PhCl, rinsing with CH2Cl2 or pentane, drying; | >99 |
In chlorobenzene W(CO)6 was refluxed with WCl6 in chlorobenzene under Ar; |
tungsten(VI) chloride
B
tungsten(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) 2 equiv. of WCl6; sealed evacuated ampoule, 200-250°C (2 h; condensation of WOCl4 in cold part), then heating to 360°C; elem. anal.; | |
stoich. mixt. heating (evac. sealed two-section ampoule, 200-250°C for 2 h, WOCl4 crystn. in cold part of ampoule), temp. raising to 360°C; thermogravimetric and differential thermal anal.; |
tungsten(IV) chloride
Conditions | Yield |
---|---|
With tetrachloromethane in closed tube at 250°C; | |
With CCl4 in closed tube at 250°C; |
Conditions | Yield |
---|---|
With chlorine | |
With Cl2 |
B
tungsten(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) Kinetics; byproducts: H2O, ethylenediamine; sample heating in N2 flow (50 ml/min) at 10 K/min between 30-800°C; TG, DTG, DSC; |
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) byproducts: ZnCl2, N2; under Ar; WCl6 and Zn3N2 in 3:1 molar ratio carefully mixed; heated at 230°C in evacuated and sealed ampoule; kept at this temp. for 1 week; cooled to 200°C in 40 h and to room temp. in 12 h; |
chlorine
A
tungsten(V) chloride
C
tungsten(VI) chloride
D
tungsten(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) Kinetics; High Pressure; linear heating rate of 5.3°C/min, Cl2(gas)-Ar(gas) flow = 4 L/h, pressure of Cl2 - 35 kPa, temperature range: 650-850°C; XRD; |
Conditions | Yield |
---|---|
In neat (no solvent) Kinetics; byproducts: O2; reaction in flow of Ar and Cl2, at temperature range 50-950°C; |
tungsten(IV) chloride
acetonitrile
trans-WCl4(MeCN)2
Conditions | Yield |
---|---|
In acetonitrile stirring (2 days); solvent removal (vac.); | 100% |
tungsten(IV) chloride
sodium chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) NaCl:WCl4=3:1, under inert atm., evacuated silica ampoule, heating up to500 °C in 5 h, keeping at this temp. for 48 h; cooling to 300 °C in 72 h, then to room temp. in 2 h; | A 99% B 0% |
N-benzyl-N,N,N-triethylammonium chloride
tungsten(IV) chloride
A
C6H5CH2N(C2H5)3(1+)*WCl6(1-)=C6H5CH2N(C2H5)3WCl6
Conditions | Yield |
---|---|
In dichloromethane react. for several days at 25°C, filtration, washing (CH2Cl2), drying (vac.), cooling of supenatant and crystn. of WCl6-salt; elem. anal.; | A 37% B 96% |
sodium benzoate
trimethylsilyl iodide
tungsten(IV) chloride
bis-diphenylphosphinomethane
Conditions | Yield |
---|---|
With Na(HBEt3) In tetrahydrofuran Ar-atmosphere; addn. of NaHBEt3 to mixt. of WCl4 and benzoate at -70°C, warming to room temp., addn. of dppm and Me3SiI, gentle heating for 24 h; washing (hexanes), solvent removal; | 94% |
tungsten(IV) chloride
Dimethyl(phenyl)phosphine
W2Cl4(P(CH3)2(C6H5))4
Conditions | Yield |
---|---|
With sodium amalgam In tetrahydrofuran under N2 sodium amalgam and Me2PPh were added to THF at -30°C followed by WCl4; shaking and warming to room temp. for ca 0.5 h; decantation, filtration through Celite; evapn., extn. with pentane, filtration, evapn., washing with MeCN, drying in vac.; elem. anal.; | 90% |
With NaB(C2H5)3H In tetrahydrofuran; toluene Ar atmosphere; addn. of soln. of NaBHEt3 in toluene to soln. of WCl4 in THF (-60°C), stirring (20 min), addn. of org. compd., slow warming (room temp., 0.5 h), stirring (12 h, room temp.); removal of solvent (vac.), dissolution in THF, filtration (Celite), pptn. on addn. of hexane, washing (hexane and MeOH), drying (vac.); | 76% |
With sodium amalgam In tetrahydrofuran 2 equiv of sodium amalgam added to a stirred soln. of WCl4 and PMe2Ph at -20°C, warmed to room temp.; filtered through Celite; elem. anal.; |
N-benzyl-N,N,N-triethylammonium chloride
tungsten(IV) chloride
(BnEt3N)[W2(μ-Cl)3Cl6]
Conditions | Yield |
---|---|
In dichloromethane stirring 1 day, filtration, evapn., crystn.; elem. anal.; | 90% |
Conditions | Yield |
---|---|
With sodium amalgam In toluene under inert atm. to mixt. WCl4 and Bu4NCl in toluene Na/Hg was added andstirred for 24 h; soln. was filtered through Celite and evapd. in vacuo, residue was dissolved in MeCN, filtered, concd. and cooled at -20°C, ppt. was filtered, recrystd. from MeCN and dried in vacuo; elem. anal.; | 90% |
Conditions | Yield |
---|---|
With n-Dodecylamine at 150 - 225℃; for 6h; Inert atmosphere; | 90% |
tungsten(IV) chloride
diphenyl(methyl)phosphine
W2(P(CH3)(C6H5)2)4Cl4
Conditions | Yield |
---|---|
With sodium amalgam In tetrahydrofuran under N2 sodium amalgam and MePPh2 were added to THF at -30°C followed by WCl4; shaking and warming to room temp. for ca 0.5 h; decantation, filtration through Celite; extn. of Celite with CH2Cl2, combining of exts. and filtrate, evapn.; elem. anal.; | 88% |
With sodium amalgam In tetrahydrofuran 2 equiv of sodium amalgam added to a stirred soln. of WCl4 and PMePh2 at -20°C, warmed to room temp.; filtered through Celite; elem. anal.; |
α-W2Cl2(1,2-bis(diphenylphosphino)ethane)2
tungsten(IV) chloride
1,2-bis-(diphenylphosphino)ethane
Conditions | Yield |
---|---|
With sodium amalgam; THF In tetrahydrofuran stirring a suspension of WCl4 with Na/Hg, -20°C, 30 min; allowing to warm to room temp.; filtration under Ar; extn. of residue with fresh THF; reducing volume of filtrate; addn. of phosphinoethane; refluxing, 15 min; stirring, room temp., 1h; reducing volume; addn. of hexane; pptn.; filtration; washing (ethanol, Et2O); elem. anal.; | 87% |
tungsten(IV) chloride
Conditions | Yield |
---|---|
With tetrahydrofuran; sodium amalgam In tetrahydrofuran under N2 WCl4 was added to THF contg. sodium amalgam; stirring for 1 h; filtration through Celite; evapn., trituration with pentane, prepd. powder was crystd. from THF/pentane; elem. anal.; | 86% |
With tetrahydrofuran; sodium amalgam In tetrahydrofuran 1 equiv of sodium amalgam added to a stirred soln. of WCl4; pentane added; |
sulfure de pentamethylene
tungsten(IV) chloride
A
Cl3W(μ-pentamethylene sulfide)3WCl3
B
[Na][Cl3W(μ-pentamethylene sulfide)2(μ-Cl)WCl3]
Conditions | Yield |
---|---|
In toluene inert atmosphere; refluxing for 45 min; cooling, pptn. on Et2O addn., extn. into CH2Cl2, then into Me2CO, repeated recrystn.; elem. anal.; | A 86% B 9.5% |
In neat (no solvent) inert atmosphere; refluxing; |
Conditions | Yield |
---|---|
With sodium amalgam In toluene under inert atm. to mixt. WCl4 and Ph4PCl in toluene Na/Hg was added andstirred for 24 h; soln. was filtered through Celite and evapd. in vacuo, residue was dissolved in MeCN, filtered, concd. and cooled at -20°C, ppt. was filtered, recrystd. from MeCN and dried in vacuo; elem. anal.; | 86% |
2,4,6-triisopropylbenzoate sodium
tungsten(IV) chloride
Conditions | Yield |
---|---|
With Na/Hg In tetrahydrofuran (N2); addn. of sodium benzoate deriv. to sodium amalgam, addn. of suspn.of tungsten compd. in dry THF at 0°C, stirring for 30 min at 0.d egree.C, warming to room temp., stirring overnight; filtration through celite, concg., keeping in cold overnight, filtration, recrystn. (THF), elem. anal.; | 86% |
Conditions | Yield |
---|---|
With sodium amalgam In tetrahydrofuran under N2 sodium amalgam and Bu3P were added to THF at -30°C followed by WCl4; shaking and warming to room temp. for ca 0.5 h; decantation, filtration through Celite; evapn., extn. with pentane, filtration, evapn., washing with MeCN, drying in vac.; elem. anal.; | 85% |
With sodium amalgam In tetrahydrofuran 2 equiv of sodium amalgam added to a stirred soln. of WCl4 and PBu3 at -20°C, warmed to room temp.; filtered through Celite; elem. anal.; |
Conditions | Yield |
---|---|
With NaBEt3H In tetrahydrofuran Ar-atmosphere; addn. of NaBEt3H to suspn. of WCl4 and benzoate at -60°C, slow warming to room temp.; filtration (Celite), washing (hexanes); | 85% |
With sodium In not given under N2 or Ar; |
depe
tungsten(IV) chloride
A
α-W2Cl4(1,2-bis(diethylphosphino)ethane)2
Conditions | Yield |
---|---|
With NaBEt3H In tetrahydrofuran Ar-atmosphere; slow addn. of excess of NaBEt3H to WCl4 at -60°C, addn. of excess of ligand at -20°C, warming to room temp., stirring overnight; pptn. on hexanes addn., filtration, washing (hexanes), drying (vac.); | A 84.7% B n/a |
With NaBEt3H; PMePh2 In tetrahydrofuran Ar-atmosphere; slow addn. of 2 equiv. of NaBEt3H to WCl4 at 0°C, addn. of 2 equiv. PMePh2, warming to room temp., addn. of excess of ligand, stirring (room temp., 2 h); pptn. on hexanes addn., filtration, washing (hexanes), drying (vac.); | A 70.6% B n/a |
Bis(diphenylphosphanyl)amine
tungsten(IV) chloride
W2Cl4(μ-bis(diphenylphosphino)amine)2
Conditions | Yield |
---|---|
With NaBH(CH2CH3)3 In tetrahydrofuran under Ar; WCl4 was suspended in THF, cooled to -60°C in EtOH/dry ice bath, NaBEt3H was added, mixt. was warmed to -20°C, soln. wasadded to the amine at room temp.; washed with hexane, remaining solvent was removed under vac.; | 81.4% |
Conditions | Yield |
---|---|
With Na#Hg In thiophene heating to boiling point of tht, stirring for 20 min in a Schlenk tube;; cooling, decantation, washing with ether, extn., recrystn.; elem. anal.;; | 81% |
With Na#Hg In thiophene stirring at 22°C for 24 h;; | 58% |
tungsten(IV) chloride
acetonitrile
tetrachlorobis(acetonitrile)tungsten(IV)
Conditions | Yield |
---|---|
In acetonitrile absence of air and moisture; stirring at room temp. for 2 d; decantation, washing (MeCN), drying (vac.); elem. anal.; | 81% |
1,4-Oxathiane
tungsten(IV) chloride
A
Cl3W(μ-1,4-thioxane)3WCl3
B
[Na][Cl3W(μ-1,4-thioxane)2(μ-Cl)WCl3]
Conditions | Yield |
---|---|
In toluene inert atmosphere; refluxing for 25 min; cooling, pptn. on Et2O addn., extn. into CH2Cl2, then into Me2CO, repeated recrystn.; elem. anal.; | A 15.3% B 81% |
In neat (no solvent) inert atmosphere; refluxing; |
Conditions | Yield |
---|---|
With tetrahydrofuran; sodium amalgam In tetrahydrofuran byproducts: sodium chloride; under Ar atm. WCl4 react. with 2 equiv. 0.4% sodium amalgam in THF at -20°C, 2 equiv. sodium benzoate added to W2Cl4(THF)4 added and stirred for 1/2 h and mixt. warmed to room temp.; soln. filtered through Celite, filtrate chilled to -20°C for 3 days; | 80% |
With C4H8O; Na#Hg In tetrahydrofuran byproducts: NaCl, Hg; (absence of air); WCl4 treated with 2 equiv of Na#Hg in THF at -20°C, sodium benzoate added, allowed to warm to room temp. with stirringfor 0.5 h; filtered, covered with hexane, crystd. for 3 d - 1 wk; | 55% |
tert-butylamine
tungsten(IV) chloride
Conditions | Yield |
---|---|
With Na/Hg; THF In tetrahydrofuran byproducts: (NH3(C(CH3)3))Cl; (N2); t-BuNH2 (43.6 mmol) added to stirred soln. of W2Cl6(THF)4 formed in situ by redn. of WCl4 (14.52 mmol) with 1 equiv. of Na/Hg (0.4%) in THF; stirring for 14 h; filtration; solvent removed (reduced pressure) from filtrate; residue extd. (hot hexane); filtration; solvent stripped from filtrate to give single crystals; elem. anal.; | 78% |
lithium dimethylamide
tungsten(IV) chloride
hexakis(dimethylamido)ditungsten(III)
Conditions | Yield |
---|---|
at 0℃; for 2h; Reflux; | 77% |
With sodium amalgam; THF In tetrahydrofuran byproducts: W(NMe2)6; 1 equiv of 1.0% Na amalgam was slowly (90 min) added to a slurry of WCl4 in THF at 0°C under N2, mixt. was stirred for 3 h at room temp., cooled to 0°C, 3 equiv of LiNMe2 was added slowly (2 h), mixt. was stirred for 12 h at room temp.; filtered through Celite (washed with THF), solvent was removed in vacuo, residue was sublimed at 120°C and 0.0001 Torr; the first isolated fraction (ca. 10%) was occasionally contaminated with small quantities of W(NMe2)6; | 75% |
In tetrahydrofuran; diethyl ether at 0℃; for 25h; Reflux; |
Conditions | Yield |
---|---|
With Na#Hg In further solvent(s) solvent: Et2S; stirring for 40 min in a Schlenk tube;; extn. with CH2Cl2, evapn.;; | 77% |
Conditions | Yield |
---|---|
With sodium amalgam In tetrahydrofuran 1 equiv of sodium amalgam added to a stirred soln. of WCl4 and PMe3; NMR; | 75% |
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