ChemicalBook CAS DataBase List 4-Iodophenylsulphur pentafluoride

4-Iodophenylsulphur pentafluoride synthesis

5synthesis methods

Product Name:4-Iodophenylsulphur pentafluoride
CAS Number:286947-68-0
Molecular formula:C6H4F5IS
Molecular Weight:330.06

To a solution of 4-(pentafluorothio)aniline (15.0 g, 68.4 mmol) and ice (40.0 g) in hydrochloric acid (12M, 30 ml) was added a solution of sodium nitrite (5.0 g, 72.5 mmol) in water (120 ml) at 0 ℃. After stirring for 2 min, the mixture was added to potassium iodide (13.0 g, 78.3 mmol) in water (120 ml), ensuring the temperature did not rise above 10 C. The reaction mixture was stirred at 0 ℃. for 10 min and then at room temperature for 60 h. The mixture was extracted with diethyl ether (2×100 ml), and the combined extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography (silica, 300 g), eluting with diethyl ether/cyclohexane [1:10]. The appropriate fractions were combined and concentrated to give 4-Iodophenylsulphur pentafluoride(16.6 g).

774-93-6 Synthesis

774-93-6
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$25.00/250mg

286947-68-0
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$45.00/50mg

Yield:286947-68-0 91%

Reaction Conditions:

with copper(l) iodide;sodium iodide;N,N`-dimethylethylenediamine in 1,4-dioxane at 110; for 24 h;Inert atmosphere;Schlenk technique;Finkelstein Reaction;

References:

Matsuzaki, Kohei;Okuyama, Kenta;Tokunaga, Etsuko;Saito, Norimichi;Shiro, Motoo;Shibata, Norio [Organic Letters,2015,vol. 17,# 12,p. 3038 - 3041] Location in patent:supporting information

2993-24-0 Synthesis