Reaktion #61480

Reaktionsgleichung

3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine

chlorosulphonic acid

→

title compound

Ausbeute 45.0%

3-Acetyl-7-chlorosulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine

Ausbeute 45.0%

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigebefore being quenched in ice/water (200 ml)
2. 2
   ExtraktionThe resulting mixture was extracted with ethyl acetate (3×100 ml)
3. 3
   Trocknendried (Na2SO4)
4. 4
   Sonstigethe solvent evaporated in vacuo

Vorschrift

A solution of 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine (4.0 g, 0.021 mol) in dichloromethane (25 ml) was added dropwise to a stirred solution of chlorosulphonic acid in dichloromethane (25 ml) at −70° C. under argon. After warming to room temperature, the reaction was stirred for 18 h before being quenched in ice/water (200 ml). The resulting mixture was extracted with ethyl acetate (3×100 ml), dried (Na2SO4) and the solvent evaporated in vacuo to give the title compound (2.74 g, 45%) as a pale yellow solid.

Quelle