Reaktion #442804

Reaktionsgleichung

2-amino-9-(4-methylphenyl)acridine

compound 12d

2-amino-9-(4-methylphenyl)acridine

methanesulfonyl chloride

diazabicyclo[2.2.2]octane

→

2-[N,N-bis(methanesulfonyl)amino]-9-(4-methylphenyl)acridine

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution heated for 2 hours
2. 2
   Temperaturunder reflux
3. 3
   Filtrationfiltration
4. 4
   workup.ADDITIONthe red filtrate added dropwise to 1000 pbv of 0.5% strength ammonia solution
5. 5
   Filtrationthe precipitate was filtered off by suction
6. 6
   Sonstigecrystallized from 135 pbv of ethanol

Vorschrift

5.68 pbw of 2-amino-9-(4-methylphenyl)acridine (compound 12d) were dissolved with 20.3 pbw of methanesulfonyl chloride and 22.4 pbw of diazabicyclo[2.2.2]octane in 120 pbv of acetonitrile and the solution heated for 2 hours under reflux. After cooling to 20° C., filtration was carried out and the red filtrate added dropwise to 1000 pbv of 0.5% strength ammonia solution. After standing overnight, the precipitate was filtered off by suction and crystallized from 135 pbv of ethanol. Yield: 1.76 pbw (20% of theory), light yellow needles. Mp.: 217°-219° C.

Quelle