CAS No.13470-13-8,TUNGSTEN TETRACHLORIDE Suppliers,MSDS download

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CAS: [13470-13-8] Molecular Weight: FW:325.66

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Synthetic route

: 7647-01-0
hydrogenchloride

: tungstic acid

: 7440-66-6
zinc

: 13470-13-8
tungsten(IV) chloride

Conditions

Conditions	Yield
strong HCl;	100%
strong HCl;	100%

...Expand

: 13283-01-7
tungsten(VI) chloride

: 13470-13-8
tungsten(IV) chloride

Conditions

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%

: phosphorous

: 13283-01-7
tungsten(VI) chloride

A: W4PCl11

B: 13470-13-8
tungsten(IV) chloride

Conditions

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%

...Expand

: 13283-01-7
tungsten(VI) chloride

: 7440-33-7
tungsten

: 13470-13-8
tungsten(IV) chloride

Conditions

Conditions	Yield
In 1,2-dichloro-ethane at 20℃; for 17h;	93%

: 7647-01-0
hydrogenchloride

: 7446-70-0
aluminium trichloride

: 13283-01-7
tungsten(VI) chloride

: 7429-90-5
aluminium

: 7647-14-5
sodium chloride

A: W6Cl8(4+)*4Cl(1-)*7H2O=[W6Cl8]Cl4*7H2O

B: 13470-13-8
tungsten(IV) chloride

Conditions

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

...Expand

: 13283-01-7
tungsten(VI) chloride

: 7440-33-7
tungsten

A: 13520-78-0, 160797-03-5
tungsten(VI) oxychloride

B: tungsten dichloride

C: 13470-13-8
tungsten(IV) chloride

Conditions

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

...Expand

: 56-23-5
tetrachloromethane

: tungsten(IV) oxide

A: tungsten(VI) oxychloride

B: 13283-01-7
tungsten(VI) chloride

C: 13470-13-8
tungsten(IV) chloride

D: 13520-76-8
tungsten dioxydichloride

Conditions

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;;

...Expand

: 13283-01-7
tungsten(VI) chloride

A: 7782-50-5
chlorine

B: 13470-13-8
tungsten(IV) chloride

Conditions

Conditions	Yield
In gas Kinetics; Irradiation (UV/VIS); stationary photolysis in a glass cell; flash photolysis in a sealed quartz cell; vac. distn.;

: 1333-74-0
hydrogen

: 13283-01-7
tungsten(VI) chloride

A: 13470-14-9
tungsten(V) chloride

B: 7782-50-5
chlorine

C: 13470-13-8
tungsten(IV) chloride

Conditions

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.;

...Expand

: 13283-01-7
tungsten(VI) chloride

: 7429-90-5
aluminium

: 13470-13-8
tungsten(IV) chloride

Conditions

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;

: 7440-33-7
tungsten

: 13470-13-8
tungsten(IV) chloride

Conditions

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 oxychloride

: 13283-01-7
tungsten(VI) chloride

A: tungsten(VI) oxychloride

B: 13470-13-8
tungsten(IV) chloride

Conditions

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.;

...Expand

: 56-23-5
tetrachloromethane

: tungsten(IV) oxide

: 13470-13-8
tungsten(IV) chloride

Conditions

Conditions	Yield
heating at 280°C in a closed tube by melting;
heating at 280°C in a closed tube by melting;

: 13283-01-7
tungsten(VI) chloride

A: 13470-14-9
tungsten(V) chloride

B: 13470-13-8
tungsten(IV) chloride

Conditions

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.;

: 14040-11-0
tungsten hexacarbonyl

: 13283-01-7
tungsten(VI) chloride

: 13470-13-8
tungsten(IV) chloride

Conditions

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(IV) oxide

: 13283-01-7
tungsten(VI) chloride

A: tungsten(VI) oxychloride

B: 13470-13-8
tungsten(IV) chloride

Conditions

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.;

...Expand

: tungsten(IV) oxide

: 13470-13-8
tungsten(IV) chloride

Conditions

Conditions	Yield
With tetrachloromethane in closed tube at 250°C;
With CCl4 in closed tube at 250°C;

: tungsten(IV) oxide

A: tungsten dioxide dichloride

B: 13470-13-8
tungsten(IV) chloride

Conditions

Conditions	Yield
With chlorine
With Cl2

: 2Cu(2+)*W(4+)*2CN(1-)*2OH(1-)*H2NC2H4NH2*2H2O*4Cl(1-)=Cu2[W(CN)2(OH)2(C2H8N2)(H2O)2]Cl4

A: copper(l) cyanide

B: 13470-13-8
tungsten(IV) chloride

Conditions

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;

: zinc nitride

: 13283-01-7
tungsten(VI) chloride

A: W2NCl8

B: 13470-13-8
tungsten(IV) chloride

Conditions

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;

...Expand

: manganese tungstate

: 7782-50-5
chlorine

A: 13470-14-9
tungsten(V) chloride

B: tungsten(VI) oxychloride

C: 13283-01-7
tungsten(VI) chloride

D: 13470-13-8
tungsten(IV) chloride

Conditions

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;

...Expand

: manganese tungstate

: 7782-50-5
chlorine

A: 13470-13-8
tungsten(IV) chloride

B: manganese(ll) chloride

Conditions

Conditions	Yield
In neat (no solvent) Kinetics; byproducts: O2; reaction in flow of Ar and Cl2, at temperature range 50-950°C;

...Expand

: 13470-13-8
tungsten(IV) chloride

: 75-05-8
acetonitrile

: 12073-20-0, 223383-17-3, 223393-83-7, 40354-88-9
trans-WCl4(MeCN)2

Conditions

Conditions	Yield
In acetonitrile stirring (2 days); solvent removal (vac.);	100%

: 13470-13-8
tungsten(IV) chloride

: 7647-14-5
sodium chloride

A: Na3[W3(μ3-Cl)(μ-Cl)3Cl9]

B: Na(1+)*W3Cl13(1-)=Na[W3Cl13]

Conditions

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%

...Expand

: 56-37-1
N-benzyl-N,N,N-triethylammonium chloride

: 13470-13-8
tungsten(IV) chloride

A: 215669-98-0
C6H5CH2N(C2H5)3(1+)*WCl6(1-)=C6H5CH2N(C2H5)3WCl6

B: 2C6H5CH2N(C2H5)3(1+)*W2Cl9(2-)=[C6H5CH2N(C2H5)3]2W2Cl9

Conditions

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%

...Expand

: 532-32-1
sodium benzoate

: 16029-98-4
trimethylsilyl iodide

: 13470-13-8
tungsten(IV) chloride

: 2071-20-7
bis-diphenylphosphinomethane

: W2(μ-O2CC6H5)2I2(μ-dppm)2 * 1/2 THF * 1/2 hexanes

Conditions

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%

...Expand

: 13470-13-8
tungsten(IV) chloride

: 672-66-2
Dimethyl(phenyl)phosphine

: 73133-21-8, 147977-45-5
W2Cl4(P(CH3)2(C6H5))4

Conditions

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.;

: 56-37-1
N-benzyl-N,N,N-triethylammonium chloride

: 13470-13-8
tungsten(IV) chloride

: 215669-96-8
(BnEt3N)[W2(μ-Cl)3Cl6]

Conditions

Conditions	Yield
In dichloromethane stirring 1 day, filtration, evapn., crystn.; elem. anal.;	90%

: 1112-67-0
tetrabutyl-ammonium chloride

: 13470-13-8
tungsten(IV) chloride

: (n-Bu4N)3[W2(μ-Cl)3Cl6]

Conditions

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%

: 34172-61-7
bis(tert-butyl) diselenide

: 13470-13-8
tungsten(IV) chloride

: tungsten(IV) selenide

Conditions

Conditions	Yield
With n-Dodecylamine at 150 - 225℃; for 6h; Inert atmosphere;	90%

: 13470-13-8
tungsten(IV) chloride

: 1486-28-8
diphenyl(methyl)phosphine

: 73133-22-9
W2(P(CH3)(C6H5)2)4Cl4

Conditions

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.;

: 73133-24-1, 73470-13-0, 86782-93-6
α-W2Cl2(1,2-bis(diphenylphosphino)ethane)2

: 13470-13-8
tungsten(IV) chloride

: 1663-45-2
1,2-bis-(diphenylphosphino)ethane

: C52H48Cl6P4W2

Conditions

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%

...Expand

: 13470-13-8
tungsten(IV) chloride

: W2Cl6(OC4H8)4

Conditions

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;

: 1613-51-0
sulfure de pentamethylene

sodium amalgam: sodium amalgam

: 13470-13-8
tungsten(IV) chloride

A: 216670-48-3
Cl3W(μ-pentamethylene sulfide)3WCl3

B: 216670-71-2
[Na][Cl3W(μ-pentamethylene sulfide)2(μ-Cl)WCl3]

Conditions

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;

...Expand

: 2001-45-8
tetraphenyl phosphonium chloride

: 13470-13-8
tungsten(IV) chloride

: (Ph4P)3[W2(μ-Cl)3Cl6]

Conditions

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%

: 1115265-86-5
2,4,6-triisopropylbenzoate sodium

: 13470-13-8
tungsten(IV) chloride

: tetrakis(2,4,6-triisopropylbenzoato)ditungsten

Conditions

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%

: 998-40-3
tributylphosphine

: 13470-13-8
tungsten(IV) chloride

: 73133-23-0
W2Cl4(P(n-Bu)3)4

Conditions

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.;

: 532-32-1
sodium benzoate

: 13470-13-8
tungsten(IV) chloride

: 110173-58-5
ditungsten(II) tetrabenzoate

Conditions

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;

: 6411-21-8
depe

: 13470-13-8
tungsten(IV) chloride

A: 205590-12-1
α-W2Cl4(1,2-bis(diethylphosphino)ethane)2

: [WOCl(1,2-bis(diethylphosphino)ethane)2]2[(WOCl4(OP(C2H5)2CH2))2]

Conditions

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

...Expand

: 2960-37-4
Bis(diphenylphosphanyl)amine

: 13470-13-8
tungsten(IV) chloride

: 264202-30-4
W2Cl4(μ-bis(diphenylphosphino)amine)2

Conditions

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%

: 110-01-0
thiophene

: 13470-13-8
tungsten(IV) chloride

: 132935-81-0
{Cl3W(μ-tetrahydrothiophene)3WCl3}

Conditions

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%

: 13470-13-8
tungsten(IV) chloride

: 75-05-8
acetonitrile

: 223383-17-3, 223393-83-7, 40354-88-9, 12073-20-0
tetrachlorobis(acetonitrile)tungsten(IV)

Conditions

Conditions	Yield
In acetonitrile absence of air and moisture; stirring at room temp. for 2 d; decantation, washing (MeCN), drying (vac.); elem. anal.;	81%

: 15980-15-1
1,4-Oxathiane

sodium amalgam: sodium amalgam

: 13470-13-8
tungsten(IV) chloride

A: 216670-42-7
Cl3W(μ-1,4-thioxane)3WCl3

B: 216670-62-1
[Na][Cl3W(μ-1,4-thioxane)2(μ-Cl)WCl3]

Conditions

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;

...Expand

: 532-32-1
sodium benzoate

: 13470-13-8
tungsten(IV) chloride

: 82752-90-7
W2(O2CC6H5)4(C4H8O)2

Conditions

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%

: 75-64-9
tert-butylamine

: 13470-13-8
tungsten(IV) chloride

: tetrachlorobis(t-butylamido)bis(t-butylamine)ditungsten(II)

Conditions

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%

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%

: 3585-33-9
lithium dimethylamide

: 13470-13-8
tungsten(IV) chloride

: 54935-70-5
hexakis(dimethylamido)ditungsten(III)

Conditions

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;

: 352-93-2
diethyl sulphide

: 13470-13-8
tungsten(IV) chloride

: {Cl3W((CH3CH2)2S)3WCl3}*CH2Cl2

Conditions

Conditions	Yield
With Na#Hg In further solvent(s) solvent: Et2S; stirring for 40 min in a Schlenk tube;; extn. with CH2Cl2, evapn.;;	77%

: 13470-13-8
tungsten(IV) chloride

: 594-09-2
trimethylphosphane

: W2Cl6(P(CH3)3)4

Conditions

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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