Reaktion #64043

Reaktionsgleichung

3-hydroxy-5-(2,4,6-trimethyl-3-chlorosulphonylphenyl)-2-propionylcyclohex-2-en-1-one

ammonia

hydrochloric acid

→

3-hydroxy-5-(2,4,6-trimethyl-3-sulfamoylphenyl)-2-propionylcyclohex-2-en-1-one

Ausbeute 81.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe product was extracted into dichloromethane (2×100 ml)
2. 2
   TrocknenThe organic layer was dried over anhydrous sodium sulphate
3. 3
   Sonstigethe solvent was removed by evaporation under reduced pressure
4. 4
   Sonstigea rotary evaporator

Vorschrift

A mixture of 3-hydroxy-5-(2,4,6-trimethyl-3-chlorosulphonylphenyl)-2-propionylcyclohex-2-en-1-one (1.3 g) and aqueous ammonia (50 ml, 25%) was stirred at 20° C. for 1 hour. The mixture was acidified with dilute hydrochloric acid and the product was extracted into dichloromethane (2×100 ml). The organic layer was dried over anhydrous sodium sulphate and the solvent was removed by evaporation under reduced pressure using a rotary evaporator to give 3-hydroxy-5-(2,4,6-trimethyl-3-sulfamoylphenyl)-2-propionylcyclohex-2-en-1-one (1.1 g, 81%) as a pale brown foam. Proton magnetic resonance spectrum (CDCl3 ;δ in ppm): 1.17 (3H, t):2.42 (3H, s); 2.63 (3H, s); 2.72 (3H, s); 2.8-4.0 (7H, m); 4.98 (2H, s); 6.96 (1H, s); 18.27 (1H, s).

Quelle