Reaktion #156245

Reaktionsgleichung

7-[3-(4-chloro-2-oxo-3-phenyl-2H-quinoline-1-yl)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

→

title compound

Ausbeute 55.9%

1-ethyl-3,3,5-trimethyl-7-[3-(2-oxo-3-phenyl-3,4-dihydro-2H-quinolin-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

Ausbeute 55.9%

Lösungsmittel

ethanol ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction mixture was subjected to celite filtration
2. 2
   Sonstigeto remove the catalyst
3. 3
   Sonstigecondensed under reduced pressure
4. 4
   SonstigeThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
5. 5
   Sonstigecondensed under reduced pressure
6. 6
   Sonstigethe residue was recrystallized from ether/hexane

Vorschrift

10% Palladium on carbon (20 mg) was added to an ethanol/ethyl acetate solution (1:1, 4 ml) of 7-[3-(4-chloro-2-oxo-3-phenyl-2H-quinoline-1-yl)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.19 g). The mixture was subjected to catalytic reduction at 50° C. under normal pressure for 6 hours. The reaction mixture was subjected to celite filtration to remove the catalyst. The filtrate was condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1). The purified product was condensed under reduced pressure, and the residue was recrystallized from ether/hexane, thereby obtaining the title compound (0.1 g) as a white powder.

Quelle