Reaktion #343791

Reaktionsgleichung

N-methyl-N-(3-tolyl)methanesulphonamide

iodine

iodic acid

sodium bicarbonate

→

N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide

Lösungsmittel

acetic acid

sulphuric acid

water

Ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   WaschenThe organic phase was washed with brine (30 ml)
2. 2
   Trocknendried (MgSO4)
3. 3
   Sonstigethe solvent evaporated

Vorschrift

A solution of N-methyl-N-(3-tolyl)methanesulphonamide (0.12 g), iodine (76 g) and iodic acid (35 mg) in glacial acetic acid (5 ml) and concentrated sulphuric acid (0.6 ml) was stirred at 80° C. for 2.5 hours. Ethyl acetate (40 ml) and water (40 ml) were then added and the mixture neutralised with solid sodium bicarbonate. The organic phase was washed with brine (30 ml), dried (MgSO4) and the solvent evaporated to leave N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide (0.22 g, 90%), m.p. 85°-87° C.

Quelle