Reaktion #340514

Reaktionsgleichung

Rongalit

2,4-dimethyl-5-mercaptoaniline

2,2,2-trifluoroethyl iodide

potassium carbonate

→

2,4-dimethyl-5-(2,2,2-trifluoroethylthio)aniline

Ausbeute 94.4%

Lösungsmittel

N,N-dimethylformamide

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate
2. 2
   TrocknenThe organic layer was dried over anhydrous magnesium sulfate
3. 3
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
4. 4
   Sonstigethe obtained residue was purified by silica gel column chromatography (eluent hexane:ethyl acetate=5:1)

Vorschrift

To a mixed solution of 20 g of 2,4-dimethyl-5-mercaptoaniline and 150 ml of N,N-dimethylformamide, 41 g of 2,2,2-trifluoroethyl iodide and 24 g of potassium carbonate were added, and 4 g of Rongalit was further added, followed by stirring at room temperature for 24 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography (eluent hexane:ethyl acetate=5:1) to obtain 29 g of 2,4-dimethyl-5-(2,2,2-trifluoroethylthio)aniline.

Quelle