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inquirytrans-(Et2O)2MoCl4
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent, solid phase) MoCl4(Et2O)2 heated under vac. in oil bath at 120°C (5 h) or 130°C (2 h); elem. anal.; | 99% |
tetrachloromethane
B
carbon dioxide
C
carbon monoxide
D
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) Kinetics; byproducts: C2Cl4; heating of Mo oxides in stream of N2 with CCl4 (560 - 800 K); reaction followed by X-ray diffraction; |
tetrachloromethane
molybdenum
A
phosgene
C
molybdenum(IV) chloride
Conditions | Yield |
---|---|
With oxygen at 310°C; |
Conditions | Yield |
---|---|
In neat (no solvent) 300°C 2d, 250°C 5 d; sublimation (100°C, vac.), extraction (dry C2Cl4); |
Conditions | Yield |
---|---|
With water In neat (no solvent) byproducts: H2, MoCl4; at 1200°C by presence of H2O;; | |
In neat (no solvent) byproducts: H2; at 1200°C;; | |
In neat (no solvent) byproducts: H2; at 1200°C;; | |
With H2O In neat (no solvent) byproducts: H2, MoCl4; at 1200°C by presence of H2O;; |
chlorine
molybdenum
A
molybdenum(V) chloride
B
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) introduction of Cl2-gas (8-9 Torr/20 min/1.8 l/h) through purified (90min/H2 stream/1000°C) Mo powder (860 - 1160°C);; extraction of MoCl5 (CCl4); extraction MoCl4 (diethylether or water); further extraction (ethanol or water);; | A n/a B 0-10 |
Conditions | Yield |
---|---|
below 500 K; |
tetrachloromethane
B
carbon dioxide
C
carbon monoxide
D
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) Kinetics; byproducts: C2Cl4; heating of Mo oxide in stream of N2 with CCl4 (560 - 800 K); reaction followed by X-ray diffraction; |
Conditions | Yield |
---|---|
In neat (no solvent) reaction on heating pulverized MoO2 with CCl4 to 250°C in a closed tube for 8h;; | 90-92 |
High Pressure; at 250°C in an autoclave, 8 h; | 90-92 |
In neat (no solvent) react. of MoO2 with CCl4 at 250°C;; | |
In neat (no solvent) react. of MoO2 with CCl4 at 250°C;; | |
In neat (no solvent) reaction on heating pulverized MoO2 with CCl4 to 250°C in a closed tube for 8h;; | 90-92 |
Conditions | Yield |
---|---|
With pyrographite mass ratio MoO2:C = 5:1; mixt. heated at 300°C in a flow of N2 loaded with CCl4; absence of moisture and oxygen; further by-product: Mo oxide chloride; removal of MoCl5 and Mo oxide chloride by vac. distn.; | A <1 B n/a |
Conditions | Yield |
---|---|
In Hexachlorobutadiene MoO2 refluxed in hexachloro-1,3-butadiene satd. with chlorine for 24 h; MoCl4 crystals obtained on cooling; | |
With tetrachloromethane In neat (no solvent) heating of powdered MoO2 with a dry mixt. of Cl2 and CCl4 at 250°C in a closed tube for several hours;; washing with CCl4; drying in vac.;; | |
With CCl4 In neat (no solvent) heating of powdered MoO2 with a dry mixt. of Cl2 and CCl4 at 250°C in a closed tube for several hours;; washing with CCl4; drying in vac.;; |
molybdenum(VI) fluoride
phosphorus trichloride
A
molybdenum(V) fluoride
phosphorus pentafluoride
C
chlorine
D
trifluorophosphane
E
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In not given react. with an excess of MoF6 forming PF3, MoCl5 and Cl2; react. of MoCl5 forming MoCl4 and Cl2; further react. of MoF6 with PF3 forming PF5 and MoF5;; | |
In not given react. with an excess of MoF6 forming PF3, MoCl5 and Cl2; react. of MoCl5 forming MoCl4 and Cl2; further react. of MoF6 with PF3 forming PF5 and MoF5;; |
tetramethylstannane
molybdenum(V) chloride
A
trimethyltin(IV)chloride
B
molybdenum(IV) chloride
Conditions | Yield |
---|---|
byproducts: CH3Cl; 2-fold excess of MoCl5; | |
byproducts: CH3Cl; 2-fold excess of MoCl5; |
tungsten(V) chloride
molybdenum(V) chloride
A
tungsten(VI) chloride
B
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) |
Conditions | Yield |
---|---|
With carbon dioxide In neat (no solvent) heating of MoCl3 in a stream of CO2 at weak red heat;; condensation of the volatile MoCl4;; | |
With carbon dioxide In neat (no solvent) heating of MoCl3 in CO2;; | |
With CO2 In neat (no solvent) heating of MoCl3 in a stream of CO2 at weak red heat;; condensation of the volatile MoCl4;; | |
With CO2 In neat (no solvent) heating of MoCl3 in CO2;; |
Conditions | Yield |
---|---|
In neat (no solvent) react. in a quartz optical cell; |
molybdenum(V) chloride
C
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In melt melting of MoCl5 and MoO2Cl2 in a closed tube;; sublimation in a stream of dry CO2; Mo2O3Cl6 as residue; volatile MoCl4;; | |
In melt melting of MoCl5 and MoO2Cl2 in a closed tube;; sublimation in a stream of dry CO2; Mo2O3Cl6 as residue; volatile MoCl4;; |
molybdenum(V) chloride
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In 1,1,2,2-tetrachloroethylene MoCl5 refluxed in tetrachloroethylene in evacuated and sealed vessel for 3 d; washed with CCl4; | |
In 1,1,2,2-tetrachloroethylene MoCl5 refluxed in tetrachloroethylene in evacuated, sealed vessel 3 d; washed with CCl4 in inert-atmosphere glove-box; |
Conditions | Yield |
---|---|
In neat (no solvent) Kinetics; byproducts: H2O, ethylenediamine; sample heating in N2 flow (60 ml/min) at 10 K/min up to 550°C; TG, DTG, DSC; |
B
molybdenum(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 |
---|---|
With Sn according to P. Stoffelbach, D. Saurenz, R. Poli, Eur. J. Inorg. Chem. (2007) 2699-2703; MoCl4(OEt2)2 dried under reduced pressure at 0°C, transferred to Schlenk flask heated for 1 h at 80°C; |
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) at 25 - 300℃; under 760.051 Torr; Inert atmosphere; |
molybdenum(IV) chloride
acetonitrile
bis(acetonitrile)tetrachloromolybdenum(IV)
Conditions | Yield |
---|---|
In acetonitrile stirring (2 days); solvent removal (vac.); | 100% |
phosphorus pentachloride
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In neat (no solvent) vac.; equimolar amts., heating (temp. gradient 250-220°C); | 100% |
molybdenum(IV) chloride
lithium tert-butoxide
Tetrakis(tert-butoxy)molybdaen(IV)
Conditions | Yield |
---|---|
In tetrahydrofuran; hexane under Ar; THF added to MoCl4, suspn. cooled (ice bath), soln. of LiOtBu in THF/hexane added with syringe, mixt. stirred for 1 h at 0°C, slowly warmed to room temp., stirred overnight; THF removed (vac.), residue extd. with pentane, then with CH2Cl2, filtered, combined extracts evapd. in vac., recrystd. from cold pentane (low yield); elem. anal.; | 99% |
Conditions | Yield |
---|---|
In tetrahydrofuran; pentane under Ar; MoCl5 suspd. in pentane, THF added, mixt. stirred for 2 min; liquid removed via cannula, residue dried; | 99% |
tellurium tetrachloride
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In melt evacuated glass ampoule: heating to 300°C for melting, after solidifying the ampoule is brought into a temp. gradient from 195 to 180°C; crystn. within some d; | 99% |
tetraethylammonium trichloro-stannate(II)
molybdenum(IV) chloride
2N(C2H5)4(1+)*MoCl4(SnCl3)2(2-)=[N(C2H5)4]2[MoCl4(SnCl3)2]
Conditions | Yield |
---|---|
In dichloromethane CH2Cl2 soln. of Sn-salt was added to suspn. of MoCl4 in CH2Cl2, mixt. was stirred for a few d under N2; filtered off, washed with CH2Cl2, dried in vac.; elem. anal.; | 98% |
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and picolinic acid (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 22 h; slurry allowed to cool and filtered, solid washed with toluene and dried in vacuo at 150°C for 20 h; elem. anal.; | A 10% B 90% |
In toluene under N2 atm. MoCl4 and picolinic acid (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 5 h; slurry allowed to cool and filtered, solid washed with toluene and dried in vacuo at 150°C for 20 h; elem. anal.; | A 30% B 70% |
2-Picolinic acid
molybdenum(IV) chloride
A
Mo(pic)4
B
Mo(NC5H4COO)3Cl
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and picolinic acid (molar ratio 1:4) in toluene heated with stirring under reflux conditions for 65 h; slurry allowed to cool and filtered, solid washed with toluene and dried in vacuo at 150°C for 20 h - Mo(pic)3Cl; filtrate reduced in volume and allowed to sit at room temp. for 24 h, ppt. collected and washed with toluene; elem. anal.; | A 2% B 88% |
Conditions | Yield |
---|---|
In neat (no solvent) absence of moisture; stirring (12 h, 20°C); filtn., crystn. (-30°C), drying (vac.), recrystn. (toluene); elem. anal.; | 82% |
dimethylacetylene
diethyl ether
molybdenum(IV) chloride
Mo(C2(CH3)2)Cl4(C2H5OC2H5)
Conditions | Yield |
---|---|
In diethyl ether under N2; slow addn. of MoCl4 to ether, addn. of alkyne, stirred for 12-16 h; filtered, dried (vac.); | 80% |
diethyl ether
hex-3-yne
molybdenum(IV) chloride
Mo(C2(C2H5)2)Cl4(C2H5OC2H5)
Conditions | Yield |
---|---|
In diethyl ether MoCl4 slowly added to Et2O, 2 equiv. of 3-hexyne added, stirred overnight; pptn.; | 80% |
In diethyl ether under N2; slow addn. of MoCl4 to ether, addn. of alkyne, stirred for 12-16 h; filtered, dried (vac.); | 80% |
Conditions | Yield |
---|---|
In diethyl ether under N2; slow addn. of MoCl4 to ether, addn. of alkyne, stirred for 12-16 h; filtered, dried (vac.); | 80% |
chloroxine
molybdenum(IV) chloride
A
chlorotris(5,7-dichloro-8-quinolinolato)molybdenum(IV)
B
dichlorobis(5,7-dichloro-8-quinolinolato)molybdenum(IV)
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 1 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.; | A 80% B 1% |
In dichloromethane under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:3) in CH2Cl2 heated with stirring under reflux conditions for 5 h; soln. filtered, ppt. extd. in Soxhlet extractor with CH2Cl2 for 18 h, residue dried in vacuo at 150°C for 20 h; elem. anal.; | A 71% B 3% |
In toluene under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:2.7) in toluene heated with stirring under reflux conditions for 4 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.; | A 60% B 10% |
In dichloromethane under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:2) in CH2Cl2 heated with stirring under reflux conditions for 3 h; soln. filtered, ppt. extd. in Soxhlet extractor with CH2Cl2 for 18 h, residue dried in vacuo at 150°C for 20 h; elem. anal.; | A 18% B 46% |
In dichloromethane under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol (molar ratio 1:3) in CH2Cl2 heated with stirring under reflux conditions for 1 h; soln. filtered, ppt. extd. in Soxhlet extractor with CH2Cl2 for 18 h, residue dried in vacuo at 150°C for 20 h; elem. anal.; | A 19% B 28% |
5-Chloro-8-hydroxyquinoline
molybdenum(IV) chloride
dichlorobis(5-chloro-8-quinolinolato)molybdenum (IV)
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and 5-chloro-8-quinolinol (molar ratio 1:2) in toluene heated with stirring under reflux conditions for 6 h; soln. filtered, solid extd. in Soxhlet extractor with CH2Cl2 for 15 h, residue dried in vacuo for 18 h at 150°C; elem. anal.; | 78% |
In toluene under N2 atm. MoCl4 and 5-chloro-8-quinolinol in toluene heated with stirring under reflux conditions for 5.5 h; soln. filtered, solid extd. in Soxhlet extractor with CH2Cl2 for 15 h, residue dried in vacuo for 18 h at 150°C; elem. anal.; | 70% |
chloroxine
molybdenum(IV) chloride
chlorotris(5,7-dichloro-8-quinolinolato)molybdenum(IV)
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and 5,7-dichloro-8-quinolinol in toluene heated with stirring under reflux conditions for 5 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.; | 74% |
molybdenum(IV) chloride
bis-[(3,4,5-trimethoxybenzyl)czclopentadienyl]molybdenum(IV) dichloride
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: LiCl; in Schlenk flask; Li compd. in THF added via cannula to THF soln. of MoCl4; refluxed for 20 h at 88°C; allowed to cool to room temp.; solvent removed under reduced pressure; washed with pentane, redissolvedin CH2Cl2, allowed to settle for 10 min; filtered through frit; solvent removed under reduced pressure, washed with pentane; elem. anal.; | 64.8% |
molybdenum(IV) chloride
riboflavine
Conditions | Yield |
---|---|
In methanol under protective gas, stirred at room temp. for 48 h; filtrated, toluene/cyclohexane added, allowed to stand at 4°C overnight, dried in high vacuum, elem. anal.; | 58% |
8-quinolinol
molybdenum(IV) chloride
A
dichlorobis(8-quinolinolato)molybdenum (IV)
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and 8-quinolinol (molar ratio 1:3) in toluene heated with stirring under reflux conditions for 4 h; soln. allowed to cool, extd. with CH2Cl2 in Soxhlet-type extractor for 144 h, residue washed with hot toluene and CH2Cl2 and dried in vacuo at 150°C for 15 h; elem. anal.; | A 51% B 23% |
2-[[(2-hydroxyphenyl)imino]methyl]phenol
molybdenum(IV) chloride
MoO(2-salicylideneaminophenolate)(DMF)
Conditions | Yield |
---|---|
With N,N-dimethyl-formamide In ethanol; N,N-dimethyl-formamide to a slurry of MoCl4 in MeOH was added a soln. of the ligand in DMF, the mixt. was stirred for a few h (N2 atm.); cooled to -20°C, solid was filtered off, washed with MeOH, dried in vac.; | 48% |
n-butyllithium
2-methylpropan-2-thiol
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In tetrahydrofuran; 1,2-dimethoxyethane n-BuLi in hexane added slowly to t-BuSH in THF at 0°C, stirred for 30 min, THF added, then added to MoCl4 in DME at 0°C, stirredfor 4 h; evapd. under vac., extd. with hexane, filtered, recrystd. from hexane at 0°C, elem.anal.; | 45% |
molybdenum(IV) chloride
bis-[(p-methoxybenzyl)cyclopentadienyl]molybdenum(IV) dichloride
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: LiCl; in Schlenk flask; Li compd. in THF added via cannula to THF soln. of MoCl4; refluxed for 20 h; allowed to cool to room temp.; solvent removed under reduced pressure; washed with pentane, redissolvedin CH2Cl2, allowed to settle for 10 min; filtered through frit; solvent removed under reduced pressure, washed with pentane; elem. anal.; | 41.5% |
nitroxoline
molybdenum(IV) chloride
A
chlorotris(5-nitro-8-quinolinolato)molybdenum(IV)
Conditions | Yield |
---|---|
In dichloromethane under N2 atm. MoCl4 and 5-nitro-8-quinolinol (molar ratio 1:3) in CH2Cl2 heated under reflux conditions with stirring for 16 h; solvent removed under vac., residue washed with hot toluene, washes combined, volume soln. reduced, soln. allowed to sit at room temp. for 24 hand filtered, product dried in vacuo at 150°C for 20 h; elem. anal.; | A 6% B 40% |
In toluene under N2 atm. MoCl4 and 5-nitro-8-quinolinol (molar ratio 1:3) in toluene heated under reflux conditions with stirring for 5 h; solvent removed under vac., residue washed with hot toluene, washes combined, volume soln. reduced, soln. allowed to sit at room temp. for 24 hand filtered, product dried in vacuo at 150°C for 20 h; elem. anal.; | A 3% B 20% |
molybdenum(IV) chloride
bis-[(3,4-dimethoxybenzyl)cyclopentadienyl]molybdenum(IV)dichloride
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: LiCl; in Schlenk flask; Li compd. in THF added via cannula to THF soln. of MoCl4; refluxed for 20 h at 88°C; allowed to cool to room temp.; solvent removed under reduced pressure; washed with pentane, redissolvedin CH2Cl2, allowed to settle for 10 min; filtered through frit; solvent removed under reduced pressure, washed with pentane; elem. anal.; | 32.3% |
2,4,6-Triisopropylthiophenol
molybdenum(IV) chloride
A
hexakis(2,4,6-triisopropylbenzenethiolato)dimolybdenum(III)
B
MoO(SC6H2(CH(CH3)2)3)4(1-)*P(C6H5)4(1+)={MoO(SC6H2(CH(CH3)2)3)4}{P(C6H5)4}
Conditions | Yield |
---|---|
With Na In 1,2-dimethoxyethane Schlenk, N2; the thiophenol in DME is treated with Na pieces, stirred at 50°C for 1 h, cooled to room temp., filtered, soln. of MoCl4 in DME is added, mixt. is stirred (room temp., 16 h), filtered (Celite), solid is washed (MeOH), Ph4PBr is added; resulting solid is the oxo product, filtrate is evapd. to dryness, residue is triturated with pentane, solid is filtered off, washed with MeOH, recrystd. (CH2Cl-MeCN); elem. anal.; | A 25% B 30% |
Conditions | Yield |
---|---|
With Na In 1,2-dimethoxyethane under N2, Schlenk technique; the thiophenol in DME is treated with Na metal pieces and stirred at 50°C for 1 h, cooled to room temp., filtered, MoCl4 is added, mixt. is stirred for 0.5 h; filtered (Celite), evapd. to dryness, extd. (hexane), recrystd. (THF-hexane); elem. anal.; | 28% |
N,N'-bis(salicylidene)-o-phenylenediamine
molybdenum(IV) chloride
dichloro(N,N'-disalicylidene-1,2-diaminobenzene)molybdenum(IV)
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and N,N'-disalicylidene-1,2-diaminobenzene in toluene heated with stirring under reflux conditions for 2 h; solvent removed under vac., residue extd. with CH2Cl2 in Soxhlet-type extractor for 24 h, residue dried in vacuo at 150°C for 24 h; elem. anal.; | 24% |
5-Chloro-8-hydroxyquinoline
molybdenum(IV) chloride
A
dichlorobis(5-chloro-8-quinolinolato)molybdenum (IV)
Conditions | Yield |
---|---|
In dichloromethane under N2 atm. MoCl4 and 5-chloro-8-quinolinol (molar ratio 1:2) in CH2Cl2 heated with stirring under reflux conditions for 3 h; soln. filtered, solid extd. in Soxhlet extractor with CH2Cl2 for 15 h, residue dried in vacuo for 18 h at 150°C; elem. anal.; | A 20% B 5% |
broxyquinoline
molybdenum(IV) chloride
chlorotris(5,7-dibromo-8-quinolinolato)molybdenum(IV)
Conditions | Yield |
---|---|
In toluene under N2 atm. MoCl4 and 5,7-dibromo-8-quinolinol in toluene heated withstirring under reflux conditions for 5 h; solvent removed under vac., residue dissolved in toluene, volume reduced and soln. allowed to sit at room temp. for 24 h, soln. filtered, ppt. washed with toluene, product dried in vacuo at 160°C for 36 h; elem. anal.; | 20% |
trithiazyl trichloride
molybdenum(IV) chloride
Conditions | Yield |
---|---|
In dichloromethane byproducts: Cl2; (exclusion of moisture); addn. of (NSCl)3 to MoCl4 in CH2Cl2 at 0-degree.C with stirring, stirring for 30 h at room temp.; filtn., cooling of the filtrate to -10°C, filtn. of the obtained crystals, washing (CH2Cl2/CCl4), drying in vac., elem. anal.; | A 9% B n/a |
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