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Conditions | Yield |
---|---|
In melt Kinetics; placing of mixt. of Ti with SnF2 (molar ratio SnF2:Ti=4.04) in Fluoroplast-4 ampule, closing by screwed stopper, exposition for 1.00 h at 230°C; various product ratio yields for various conditions; cooling, stirring up in water, collection, drying; | A 13.8% B n/a |
Conditions | Yield |
---|---|
In hydrogen fluoride reaction of ClF3 with Ti in HF-suspension at -78°C;; | |
In hydrogen fluoride HF (liquid); reaction of ClF3 with Ti in HF-suspension at -78°C;; |
Conditions | Yield |
---|---|
With hydrogen fluoride In water byproducts: H2; at room temp.; | |
With fluorine gentle heating; | |
With hydrogen fluoride byproducts: H2; at red heat; |
Conditions | Yield |
---|---|
In hydrogen fluoride | |
100-120°C; | |
HF free of water;; |
titanium(III) fluoride
hydrogen fluoride
A
hydrogen
B
titanium(IV) fluoride
Conditions | Yield |
---|---|
In water Kinetics; |
Conditions | Yield |
---|---|
Kinetics; 220 to 400°C, 0.2 to 1 atm HF; |
Conditions | Yield |
---|---|
Kinetics; byproducts: oxide, fluorides; => 200°C; | |
With sulfuric acid In water | 0% |
Conditions | Yield |
---|---|
byproducts: HCl; vigorous reaction; | |
byproducts: HCl; vigorous reaction; |
Conditions | Yield |
---|---|
With boron trifluoride at 500°C; | |
With BF3 at 500°C; |
Dichlorodifluoromethane
B
titanium(IV) fluoride
C
titanium tetrachloride
Conditions | Yield |
---|---|
In neat (no solvent) reaction at 700-750°C;; |
Conditions | Yield |
---|---|
byproducts: H2; red heat; |
Conditions | Yield |
---|---|
With Ar In neat (no solvent) at 150°C for 2 d; | |
In neat (no solvent) |
titanium(IV) fluoride
Conditions | Yield |
---|---|
With F2; Ar In hydrogen fluoride HF (liquid); 300°C, 1 d, cooling (20°C/d to room temp., 3 weeks); |
barium fluorotitanate
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: BaF2; glowing; |
chloryl fluoride
titanium tetrachloride
B
chlorine dioxide
C
chlorine
D
titanium(IV) fluoride
Conditions | Yield |
---|---|
In neat (no solvent) at -100°C;; |
uranium hexafluoride
titanium tetrachloride
A
uranium(IV) tetrafluoride
B
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: Cl2; UF6 in excess; | |
byproducts: Cl2; UF6 in excess; |
uranium hexafluoride
titanium tetrachloride
A
uranium hexachloride
B
uranium(IV) tetrafluoride
C
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: Cl2; TiCl4 in excess; | |
byproducts: Cl2; TiCl4 in excess; |
uranium hexafluoride
titanium tetrachloride
A
uranium hexachloride
B
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: Cl2, UF4; TiCl4 in excess; | |
byproducts: Cl2, UF4; TiCl4 in excess; |
β-uranium(V) fluoride
titanium tetrachloride
A
uranium hexachloride
B
uranium(IV) tetrafluoride
C
titanium(IV) fluoride
Conditions | Yield |
---|---|
heating in N2-stream, NH4F evolution above 100°C, TiF4-loss from 150°C; | |
heating in N2-stream, NH4F evolution above 100°C, TiF4-loss from 150°C; |
titanium oxyfluoride
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: TiO2; by heating; |
Conditions | Yield |
---|---|
decompn. at 600°C; |
titanium(IV) fluoride
Conditions | Yield |
---|---|
With boron trifluoride 500°C; | |
With BF3 |
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: F2; above 900°C; | |
byproducts: F2; above 900°C; |
TiF4*C5H5N
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: C5H5N; heating in moist. air; |
titanium(IV) fluoride
Conditions | Yield |
---|---|
very strong heating; | |
very strong heating; |
titanium(IV) fluoride
Conditions | Yield |
---|---|
With hydrogen fluoride In water byproducts: H2O2; | |
With HF In water |
titanium(IV) fluoride
Conditions | Yield |
---|---|
byproducts: H2O; at 300°C; | |
byproducts: H2O; at 300°C; |
titanium
fluorine
A
titanium(III) fluoride
D
titanium(IV) fluoride
Conditions | Yield |
---|---|
In solid matrix Irradiation (UV/VIS); Ti atoms evapd., trapped in F2/Ar matrix at ca 10 K, photolyzed using Hg-Xe, annealed to 25 K; not isolated, detected by IR; |
Conditions | Yield |
---|---|
In hydrogen fluoride HF (liquid); |
Conditions | Yield |
---|---|
In acetonitrile at -196 - 20℃; for 8h; | 100% |
Conditions | Yield |
---|---|
In acetonitrile at -196 - 20℃; for 16h; | 100% |
1,2-bis(dimethylphosphanyl)ethane
titanium(IV) fluoride
acetonitrile
(TiF4((CH3)2PCH2CH2P(CH3)2))
Conditions | Yield |
---|---|
In dichloromethane (N2) TiF4 was dissolved in MeCN, soln. was filtered and evapd. in vacuo,residue was dissolved in CH2Cl2, ligand was added dropwise, stirred for 2 h; solvent was removed in vacuo, residue was washed with hexane, filtered off and dried in vacuo; elem. anal.; | 91% |
Conditions | Yield |
---|---|
In acetonitrile soln. of (15)crown-5 in MeCN added to soln. of TiF4 in MeCN; concd., stored at room temp. for several h; elem. anal.; | 90% |
titanium(IV) fluoride
1,3,4,5-tetramethylimidazol-2-ylidene
Conditions | Yield |
---|---|
In tetrahydrofuran (N2); addn. of THF soln. of titanium fluoride to THF soln. of imidazole deriv. at -79°C, stiring for 30 min at -79°C, warming to room temp., stirring for 6 h at room temp.; filtration, washing with THF, drying in vac., recrystn. (CH2Cl2), elem. anal.; | 90% |
dichloromethane
1,2-bis(dimethylphosphino)benzene
titanium(IV) fluoride
acetonitrile
Conditions | Yield |
---|---|
In dichloromethane (N2) TiF4 was dissolved in MeCN, soln. was filtered and evapd. in vacuo,residue was dissolved in CH2Cl2, ligand was added dropwise, stirred for 1 h; solvent was removed in vacuo, residue was triturated with hexane and stirred for 2 h, ppt. was filtered off and dried in vacuo; elem. anal.; | 85% |
Conditions | Yield |
---|---|
In dichloromethane dry N2-atmosphere; refluxing for 6 h; elem. anal.; | 84% |
titanium(IV) fluoride
Conditions | Yield |
---|---|
In dichloromethane TiF4 refluxed in CH2Cl2 with the organic compound for 12 h, soln. cooled; filtered, concentrated under a stream of N2, hexane added, recrystd. from CH2Cl2-hexane; elem. anal.; | 83% |
titanium(IV) fluoride
Ti(CH3COCHCOCH3)2F2
Conditions | Yield |
---|---|
In n-heptane; 1,2-dichloro-ethane at 20℃; Schlenk technique; Inert atmosphere; | A 81% B n/a |
Conditions | Yield |
---|---|
In acetonitrile under N2; solns. of TiF4 in MeCN, 15-crown-5 in MeCN and SbF5 (molar ratio 1:1:2.4) in MeCN mixed at room temp.; filtered; concd.; left at 5°C for 5 d; filtered; crystals washed with cold (-20 to -40°C) CH2Cl2; elem. anal.; | 80% |
Conditions | Yield |
---|---|
With BuLi In hexane; toluene byproducts: LiF; (N2); addn. of soln. of BuLi in hexane to soln. of propanol deriv. in toluenen at -78°C, stirring at -78°C for 1 h and at room temp. for 1 h, addn. to suspn. of titanium compd. in toluene at room temp.,stirring for 2 h, refluxing for 1 d; filtration, extn. (hexane), filtration, concn., keeping for 5 d at 5°C, filtration, elem. anal.; | 80% |
1,2-dimethoxyethane
titanium(IV) fluoride
(κ2-1,2-dimethoxyethane)tetrachlorotitanium(IV)
Conditions | Yield |
---|---|
In dichloromethane (Ar), TiF4 in CH2Cl2 treated with 1 equiv. of ligand, stirred at room temp. for 4 h; evapd.(vac.), elem. anal.; | 80% |
titanium(IV) fluoride
Ti(CH3COCHCOCH3)2F2
Conditions | Yield |
---|---|
In 1,2-dichloro-ethane at 20℃; Schlenk technique; Inert atmosphere; | A 78% B 80% |
Conditions | Yield |
---|---|
In acetonitrile under N2 atm. soln. TiF4 in MeCN was added soln. Ti(NMe2)4 in MeCN at room temp. and stirred for 30 min; ppt. was filtered, washed with MeCN, and dried in vacuo overnight; elem.anal.; | 75% |
antimony pentafluoride
titanium(IV) fluoride
acetonitrile
fac-trifluorotris(acetonitrile)titanium(IV) hexafluoroantimonate(V)*(acetonitrile)
Conditions | Yield |
---|---|
In acetonitrile under N2; SbF5 (1 equiv.) distd. under vac.; MeCN condensed onto SbF5 at-79°C; warmed; added to soln. of TiF4 (1 equiv.) in MeCN at room temp.; filtered; concd.; left at 5°C for 5 d; filtered; crystals washed with cold (-20 to -40°C) CH2Cl2; elem. anal.; | 70% |
In acetonitrile under N2; SbF5 (2 or 3 equiv.) distd. under vac.; MeCN condensed onto SbF5 at -79°C; warmed; added to soln. of TiF4 (1 equiv.) in MeCN atroom temp.; filtered; concd.; left at 5°C for 5 d; filtered; crystals washed with cold (-20 to -40°C) CH2Cl2; |
Conditions | Yield |
---|---|
In tetrahydrofuran (N2) soln. TiF4 in THF was stirred for 30 min; soln. was filtered, concd. in vacuo and refrigerated for 24 h, ppt. was filtered off and dried in vacuo; elem. anal.; | 69% |
Schlenk technique; Glovebox; Inert atmosphere; |
Conditions | Yield |
---|---|
In dichloromethane (N2) TiF4 was dissolved in MeCN, soln. was filtered and evapd. in vacuo,residue was dissolved in CH2Cl2, ligand was added dropwise, stirred for 2 h; solvent was removed in vacuo, residue was stirred overnight with hexane and CH2Cl2, ppt. was filtered off and dried in vacuo; elem. anal.; | 68% |
5,11,17,23,29,35-hexakis(tert-butyl)-37,38,39,40,41-hexakis(hydroxy)calix[6]arene
titanium(IV) fluoride
acetonitrile
Conditions | Yield |
---|---|
Stage #1: 5,11,17,23,29,35-hexakis(tert-butyl)-37,38,39,40,41-hexakis(hydroxy)calix[6]arene; titanium(IV) fluoride In toluene for 12h; Reflux; Inert atmosphere; Stage #2: acetonitrile at 0℃; for 48h; Inert atmosphere; | 68% |
Conditions | Yield |
---|---|
In dichloromethane at 24.84℃; for 30h; Schlenk technique; Reflux; Inert atmosphere; | 66% |
N-tris(pentafluorobenzyl)-B-trichloroborazine
titanium(IV) fluoride
N-tris(pentafluorobenzyl)-B-trifluoroborazine
Conditions | Yield |
---|---|
64% | |
64% |
titanium(IV) fluoride
lithium hexamethyldisilazane
fluoro-tris(bis-trimethylsilyl-amido)titanum
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: LiF; Ar; stoichiometric amounts; room temperature; stirring for 1 d;; evapn. to dryness; addn. of hexane; filtration on celite; solvent concentration; crystn. upon cooling to -30 ° C; ekem. anal.;; | 60% |
Conditions | Yield |
---|---|
In acetonitrile under N2; solns. of TiF4 in MeCN, 18-crown-6 in MeCN and SbF5 (molar ratio 1:1:3) in MeCN mixed at room temp.; filtered; concd.; left at 5°C for 5 d; filtered; crystals washed with cold (-20 to -40°C) CH2Cl2; elem. anal.; | 60% |
Conditions | Yield |
---|---|
In dichloromethane dry N2-atmosphere; refluxing for 5.5 h; elem. anal.; | 60% |
p-methyl-N,N'-dimethyldiazacalix[3.1.1.3.1.1]arene
titanium(IV) fluoride
acetonitrile
Conditions | Yield |
---|---|
Stage #1: p-methyl-N,N'-dimethyldiazacalix[3.1.1.3.1.1]arene; titanium(IV) fluoride In toluene for 12h; Inert atmosphere; Schlenk technique; Reflux; Stage #2: acetonitrile Inert atmosphere; Schlenk technique; | 56% |
Conditions | Yield |
---|---|
stirring for 1 h; distn.; | 54% |
stirring for 1 h; distn.; | 54% |
B-trichloro-N-triphenylborazine
titanium(IV) fluoride
2,4,6-trifluoro-1,3,5-triphenyl-borazine
Conditions | Yield |
---|---|
52% | |
52% |
Conditions | Yield |
---|---|
In further solvent(s) byproducts: FCH(CH3)2; addn. of phosphine oxide to soln. of Ti-halide in heptadecane, heating (N2-atmosphere, 300°C), rapid addn. of 1 equiv. of Ti-alkoxide, 5 min; centrifugation, washing (acetone); XRD pattern characterisation; | 50% |
Conditions | Yield |
---|---|
In acetonitrile Schlenk techique, under N2; CH3CN condenced into mixt. of TiF4 (6.5 mmol) + 18-crown-6 (3.0 mmol) (-79°C); warmed to 50°C; filtered; concd.; kept (room temp., 5 d); crystals filtered; washed withCH2Cl2 (from -20 to -40°C); elem. anal.; | 50% |
Conditions | Yield |
---|---|
With MeLi In tetrahydrofuran; diethyl ether byproducts: LiF; (N2); addn. of soln. of 2 equiv. of MeLi in ether to soln. of 2 equiv. of propanol deriv. in THF at -78°C, stirring at -78°C for 1h and at room temp., addn. to soln. of titanium compd. in THF at room t emp., stirring for 2 h; evapn., keeping at room temp. for 2 d; first product: filtration, washing with CH2Cl2, drying in vac., elem. anal.; second product: evapn. of filtrate, extn. (hexane), filtration, concn., keeping for 5 d at 5°C, filtration, elem. anal.; | A n/a B 50% |
With MeLi In tetrahydrofuran; diethyl ether byproducts: LiF; (N2); addn. of soln. of 3 equiv. of MeLi in ether to soln. of 3 equiv. of propanol deriv. in THF at -78°C, stirring at -78°C for 1h and at room temp., addn. to soln. of titanium compd. in THF at room t emp., stirring for 2 h; evapn., keeping at room temp. for 2 d; first product: filtration, washing with CH2Cl2, drying in vac., elem. anal.; second product: evapn. of filtrate, extn. (hexane), filtration, concn., keeping for 5 d at 5°C, filtration, elem. anal.; | A 40% B 30% |
Conditions | Yield |
---|---|
C6H5BBr2 + TiF4 mixed to a pulp, after 15 min stirring it liquefies, boiled using backflow for 2 h; distn.; | 49% |
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