Reaktion #605703

Reaktionsgleichung

HCl

Ethylsulfonyl chloride

3-bromo-5-(2,4-difluorophenoxy)aniline

pyridine

→

title compound

Ausbeute 95.6%

N-[3-bromo-5-(2,4-difluorophenoxyl)phenyl]ethanesulfonamide

Ausbeute 95.6%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with DCM (3×5 mL)
2. 2
   Waschenthe combined organic extracts were washed with saturated bicarbonate solution (aq)
3. 3
   Trocknendried over sodium sulfate
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated in vacuo
6. 6
   SonstigeThe crude solid was purified by silica gel column chromatography

Vorschrift

Ethylsulfonyl chloride (15 uL, 0.16 mmol) was added dropwise to a stirred solution of 3-bromo-5-(2,4-difluorophenoxy)aniline (48 mg, 0.16 mmol) and pyridine (40 uL, 0.48 mmol) in DCM (320 uL) at 0° C. under nitrogen. After the mixture was allowed to warm to rt and stir for 12 h, it was treated with 1N HCl (1 mL) and extracted with DCM (3×5 mL); the combined organic extracts were washed with saturated bicarbonate solution (aq), dried over sodium sulfate, filtered and concentrated in vacuo. The crude solid was purified by silica gel column chromatography using a gradient of EtOAc (5 to 60%) in hexanes to afford the title compound (60 mg, 95%) as a tan solid. LCMS (M+H)+=393.

Quelle