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4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride

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4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride Basic information

Product Name:
4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride
Synonyms:
  • 4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride
  • 4-(tert-Butyl)-2,6-dimethylphenylsulphur trifluoride
  • Fluolead, 5-(tert-Butyl)-1,3-dimethyl-1-(trifluorothio)benzene
  • FLUOLEAD(TM)
  • 4-tert-Butyl-2,6-dimethylphenylsulphur trifluoride ,90%
  • Fluolead, 5-(tert-Butyl)-1,3-dimethyl-2-(trifluorothio)benzene
  • 2,6-Dimethyl-4-tert-butylphenylsulfur trifluoride
  • Fluolead
CAS:
947725-04-4
MF:
C12H17F3S
MW:
250.32
Mol File:
947725-04-4.mol
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4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride Chemical Properties

Melting point:
62-68 °C
Boiling point:
92-93℃ (0.5 Torr)
Density 
1.07±0.1 g/cm3(Predicted)
storage temp. 
0-10°C
form 
crystal
color 
white to off-white
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Safety Information

Hazard Codes 
T
Risk Statements 
14-25-34
Safety Statements 
26-36/37/39-45
RIDADR 
UN 2923 6.1(8) / PGI
WGK Germany 
3
TSCA 
No
HazardClass 
8
PackingGroup 
II
HS Code 
29309090
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4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride Usage And Synthesis

Chemical Properties

White powder

Uses

Air and thermally stable alternative to DAST. Efficient deoxofluorinating agent for a wide variety of substrates.

Uses

Features:

  • Tolerance of many functional groups
  • Highly selective functionalization
  • Highly efficient and broad reaction scope
  • Mild reaction conditions

Generally superior reactivity and selectivity to SF4 and easier and safer to handle.

Shown to promote nucleophilic deoxofluorination reactions and exhibits excellent thermal stability, up to 150 °C, therefore rendering it safely applicable in a variety of processes, including industrial scale production.


Novel fluorinating reagent applicable to a variety of chemical processes (Scheme 1).

Refer to the Datasheet for more information on Fluolead?: A Novel New Versatile Fluorinating Agent

Uses

4-tert-Butyl-2,6-dimethylphenylsulfur Trifluoride is a deoxofluorination reagent used in an improved method of synthesis of arylsulfur trifluorides.

General Description

4-tert-Butyl-2,6-dimethylphenylsulfur trifluoride is a thermally stable, easy-to-handle, versatile deoxofluorinating agent that also shows high stability on contact with water. It is a superior alternative to diethylaminosulfur trifluoride (DAST).

Synthesis

68819-90-9

947725-04-4

The general procedure for the synthesis of 4-tert-butyl-2,6-dimethylphenyl sulfur trifluoride (Fluolead) from 1,2-bis(4-(tert-butyl)-2,6-dimethylphenyl) disulfide was as follows: in a flame-dried 500 mL round-bottom flask equipped with a dropping funnel, anhydrous acetonitrile (120 mL) was added and operated under nitrogen protection. Under stirring conditions, spray-dried potassium fluoride (29.1 g, 500 mmol) and bis(2,6-dimethyl-4-tert-butylphenyl) disulfide (19.4 g, 50 mmol) were added sequentially. Subsequently, the reaction mixture was cooled to 0 °C by an ice bath and bromine (26 mL, 500 mmol) was added slowly and dropwise. After the dropwise addition, the reaction mixture was continued to be stirred at 0 °C for 2 hours. After completion of the reaction, the solvent and excess bromine were removed under reduced pressure at room temperature. Finally, the product was purified by distillation under reduced pressure to give 17.5 g of light white solid in 70% yield. The product was characterized by 19FNMR (d-CH3CN): δ50.9 (t, J=62.7 Hz, 2F), -58.4 (d, J=62.7 Hz, 1F).

References

[1] Patent: US2012/83627, 2012, A1. Location in patent: Page/Page column 2
[2] Journal of the American Chemical Society, 2010, vol. 132, # 51, p. 18199 - 18205
[3] Patent: US7265247, 2007, B1. Location in patent: Page/Page column 11
[4] Patent: WO2008/13550, 2008, A1. Location in patent: Page/Page column 12
[5] Patent: US7265247, 2007, B1. Location in patent: Page/Page column 12

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