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inquiryImidodisulfurylfluoride CAS NO.14984-73-7 Application:Imidodisulfurylfluoride CAS NO.14984-73-7
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inquiry1,1,1,3,3,3-hexamethyl-disilazane
A
trimethylsilyl fluoride
B
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With fluorosulfonyl fluoride In acetonitrile at 20 - 90℃; for 3h; Autoclave; | A n/a B 98% |
bis(chlorosulfonyl)amine
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With perfluorooctylsulfonyl fluoride; hydrogen fluoride at 65 - 70℃; for 15h; Time; | 95.3% |
With hydrogen fluoride; dimethyl sulfate at 90℃; for 16h; Reagent/catalyst; Inert atmosphere; | 90% |
With zinc(II) fluoride In acetic acid butyl ester at 25℃; for 6h; Product distribution / selectivity; Inert atmosphere; | 79% |
1,1,1,3,3,3-hexamethyl-disilazane
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With fluorosulfonyl fluoride In ethyl acetate at 100℃; for 3h; Solvent; Temperature; Autoclave; | 95% |
Conditions | Yield |
---|---|
at 20℃; for 12h; Concentration; Inert atmosphere; | 90% |
at 20 - 50℃; | Ca. 93 g |
Conditions | Yield |
---|---|
With chlorosulfonic acid; isocyanate de chlorosulfonyle at 160℃; under 60006 Torr; for 0.25h; Reagent/catalyst; Temperature; Pressure; Time; | 89% |
at 130℃; for 2h; Product distribution / selectivity; Autoclave; | 55% |
fluorosulphonic acid
urea
A
sodium fluorosulfonate
B
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With sodium chloride In dichloromethane distn. of a react.-mixt. of urea and HSO3F under vac.; distillate dissolved in CH2Cl2; NaCl added; stirred for 6 h under reflux;; NaSO3F filtered off; filtrate cooled to -80°C; filtn., recrystn. (CFCl3, -80°C).; | A n/a B 87.8% |
Conditions | Yield |
---|---|
Stage #1: bis(chlorosulfonyl)amine; zinc(II) fluoride In acetic acid butyl ester at 25℃; for 6h; Inert atmosphere; Stage #2: ammonia In acetic acid butyl ester; water Product distribution / selectivity; | A n/a B 81% |
chlorosulfonic acid
aminosulfonic acid
thionyl fluoride
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In 1,2-dichloro-ethane at 80℃; under 16501.7 Torr; for 17h; Solvent; Autoclave; | 77% |
bis(chlorosulfonyl)amine
antimony(III) fluoride
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In neat (no solvent) absence of air and moisture; slight excess amine, stirring for 4 h; fractional distn. (25°C, 0.01 Torr), decantation from residual SbCl3; | 70% |
fluorosulphonic acid
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In neat (no solvent) under dry N2; KN(SO2F)2 placed in dry Schlenk vessel and HSO3F added under stream of dry nitrogen; mixture stirred with a glass stick and allowed to stay for one hour; HN(SO2F)2 distilled off under vacuum; contains small amounts of HSO3F according to (19)F-NMR; | 62% |
fluorosulfonyl fluoride
aminosulfonic acid
fluorosulphonic acid
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In 1,2-dichloro-ethane at 92℃; under 27752.8 Torr; for 10h; Solvent; Autoclave; | 53% |
thionyl chloride
fluorosulphonic acid
urea
A
imido-bis(sulfuric acid) fluoride chloride
B
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In thionyl chloride under dry N2; urea placed into a flask and flask immersed to a cold water bath; thionyl chloride added; HSO3F added dropwise, then the flask fitted with a reflux condenser, connected to a CaCl2 drying tube; heated at110°C for 42 h; reaction mixture fractionally distilled under vacuum; main fraction collected in the range 45-65°C/650 Pa; mixture of HN(SO2F)2, HN(SO2Cl)(SO2F), HSO3F in a ratio of 2.9:2.3:1 according to (19)F-NMR; |
thionyl chloride
aminosulfonic acid
fluorosulphonic acid
A
imido-bis(sulfuric acid) fluoride chloride
B
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In thionyl chloride amidosulfuric acid placed into a flask and thionyl dichloride added under dry argon; HSO3F added dropwise, then the flask fitted with a reflux condenser, connected to a CaCl2 drying tube; heated at 120°C for 38 h; reaction mixture fractionally distilled under vacuum; main fraction collected in the range 47-80°C/650 Pa; mixture of HN(SO2F)2, HN(SO2Cl)(SO2F), HSO3F in a ratio of 4.8:10.5:1 according to (19)F-NMR; |
fluorosulfonyl isocyanate
fluorosulphonic acid
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In not given byproducts: CO2; distilled; |
Conditions | Yield |
---|---|
In acetonitrile at 25℃; for 24h; |
fluorosulfonyl fluoride
ammonia
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With N,N,N'N'-tetramethyl-1,3-propanediamine In acetonitrile at 11 - 25℃; under 123 - 760 Torr; for 13h; Product distribution / selectivity; Industry scale; |
Conditions | Yield |
---|---|
at 120℃; Large scale; |
Conditions | Yield |
---|---|
In dichloromethane at 0 - 20℃; Schlenk technique; Inert atmosphere; | 100% |
tetramethylstannane
bis(fluorosulfonyl)amide
trimethyltin(IV) di(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In dichloromethane N2 atm.; equimolar ratio, refluxing (4 h); evapn.; elem. anal.; | 97% |
bis(fluorosulfonyl)amide
cyhexatin
tricyclohexyltin(IV)-di(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With Na2SO4 In dichloromethane N2 atm.; equimolar ratio, stirring (1 h); filtn., evapn. (vac.); elem. anal.; | 97% |
Conditions | Yield |
---|---|
In trichlorofluoromethane dropwise addn. of CFCl3 to HN(SO2F)2 (exclusion of moisture), NH3 flow is passed into this soln. at room temp. until ppt. dissolves; evapn. under reduced pressure, washing with CFCl3, elem. anal.; | 96.5% |
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
With lithium acetate; acetic acid at 0 - 5℃; for 4h; Reagent/catalyst; | 94.9% |
With lithium hydroxide In water Product distribution / selectivity; | 90% |
With lithium fluoride; carbonic acid dimethyl ester at 0 - 5℃; for 3h; Reagent/catalyst; |
zinc(II) trifluoroacetate
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In trifluoroacetic acid byproducts: CF3COOH; Excess of HN(SO2F)2 is added to Zn(OOCCF3)2, the mixture is refluxed for 16 h.; compd. is filtered, washed with CF3COOH, CH2Cl2, dried in vacuo at 80°C, elem. anal.; | 92% |
lithium carbonate
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In water at -78 - 20℃; pH=7; | 92% |
In water pH=7; |
cobalt trifluoroacetate
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In trifluoroacetic acid Addn. of excess HN(SO2F)2 to Co(O2CCF3) soln. under N2, refluxing (14 h), pink solid forms.; Filtn. under positive N2 pressure, washing (trifluoroacetic acid, CH2Cl2), drying in vac., elem. anal.; | 91% |
Tetramethylblei-(IV)
bis(fluorosulfonyl)amide
trimethyllead(IV)-di(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In dichloromethane N2 atm.; refluxing (3 h); evapn., recrystn. (CH2Cl2/petroleum ether 3/1); elem. anal.; | 87% |
xenon difluoride
bis(fluorosulfonyl)amide
fluoro[imidobis(sulfuryl fluoride)]xenon(II)
Conditions | Yield |
---|---|
In Dichlorodifluoromethane byproducts: HF; HN(SO2F)2 syringed onto vessel with XeF2 cooled to -196°C, dry CF2Cl2 condensed onto sample at -196°C, warmed to 0°C with vigorously agitation, when formed HF extd. into upper CF2Cl2 layer, mixt. stood for 1 d at 0°C; volatiles removed in vac. at 0°C, tube and contents allowed to warm to room temp., pumped; | 86% |
bis(fluorosulfonyl)amide
fluoro[imidobis(sulfuryl fluoride)]xenon(II)
Conditions | Yield |
---|---|
With CF2Cl2 liquid HN(SO2F)2 was syringed onto XeF2 at -196°C, then CF2Cl2 was condenced on to the sample and warmed to 0°C with vogorous agitation for 1 day, when HF was exctrated into upper CF2Cl2 layer; CF2Cl2 and HF were removed in vac. at 0°C, a residue was warmed to room temp. and XeF2 was removed in vac.; | 86% |
xenon difluoride
bis(fluorosulfonyl)amide
A
fluoro[imidobis(sulfuryl fluoride)]xenon(II)
B
hydrogen fluoride
Conditions | Yield |
---|---|
In Dichlorodifluoromethane 3 d at 0°C, 1:1 molar ratio; The reactor was pumped for 3 h at 0°C to remove the byproducts, elem. anal.; | A 80% B n/a |
bis(fluorosulfonyl)amide
lithium hydroxide
Conditions | Yield |
---|---|
In isopropyl alcohol at 20℃; for 7h; | 73% |
tetramethylgermane
bis(fluorosulfonyl)amide
trimethylgermyl-di(fluorosulfonyl)amine
Conditions | Yield |
---|---|
In dichloromethane N2 atm.; 18 h, 20°C; evapn., distn. (vac.); elem. anal.; | 63% |
Tetraphenyllead
bis(fluorosulfonyl)amide
triphenyllead(IV)-di(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In dichloromethane N2 atm.; equimolar ratio, refluxing (2 d); filtn., evapn., washing (CCl4), drying (vac.); elem. anal.; | 43% |
xenon difluoride
bis(fluorosulfonyl)amide
A
Xe[N(SO2F)2]2
B
hydrogen fluoride
Conditions | Yield |
---|---|
In Dichlorodifluoromethane byproducts: [N(SO2F)2]2, SO2F2, HF; 2 weeks from -22°C to -12°C, 2:1 molar ratio; The reactor was pumped at -4°C to remove the byproducts, elem. anal.; | A 20% B n/a |
cadmium(II) trifluoroacetate
bis(fluorosulfonyl)amide
Conditions | Yield |
---|---|
In trifluoroacetic acid byproducts: CF3COOH; Excess of HN(SO2F)2 is added to Cd(OOCCF3)2, the mixture is refluxed for 16 h.; compd. is filtered, washed with CF3COOH, CH2Cl2, dried in vacuo at 80°C, elem. anal.; | >90 |
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