Reaktion #466608

Reaktionsgleichung

N-tert.-butyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide

methanesulfonic acid

→

6-morpholin-4-yl-4-o-tolyl-nicotinamide

Ausbeute 96.8%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONpoured on ice
2. 2
   ExtraktionThe aqueous phase was extracted with tert.-butyl-methylether
3. 3
   Extraktionextracted further with tert.-butyl-methylether
4. 4
   TrocknenThe second organic extracts were dried (Na2SO4)
5. 5
   Einengenconcentrated

Vorschrift

A mixture of 6.0 g (16.5 mMol) N-tert.-butyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide and 12 ml (185 mMol) methanesulfonic acid was stirred at 100° C. for 5 hours, then poured on ice. The aqueous phase was extracted with tert.-butyl-methylether, brought to pH =10 with NaOH aq. 28% and extracted further with tert.-butyl-methylether. The second organic extracts were dried (Na2SO4) and concentrated to yield 4.75 g (96%) 6-morpholin-4-yl-4-o-tolyl-nicotinamide as a light beige crystalline foam.

Quelle