Reaktion #156246

Reaktionsgleichung

7-[3-(2,3-Dioxo-2,3-dihydroindol-1-yl)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

Water

→

title compound

Ausbeute 61.9%

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

Ausbeute 61.9%

Lösungsmittel

hydrazine hydrate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile heated
2. 2
   Temperaturunder reflux
3. 3
   Extraktionfollowed by extraction by ethyl acetate
4. 4
   TrocknenThe organic layer was dried by anhydrous sodium sulfate, and condensed under reduced pressure
5. 5
   SonstigeThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=85:15)
6. 6
   Sonstigecondensed under reduced pressure
7. 7
   Sonstigethe residue was recrystallized from ether/hexane

Vorschrift

7-[3-(2,3-Dioxo-2,3-dihydroindol-1-yl)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.3 g) was suspended in hydrazine hydrate (3 ml), and the liquid was stirred for two hours while heated under reflux. The reaction mixture was cooled to room temperature. Water was added thereto, followed by extraction by ethyl acetate. The organic layer was dried by anhydrous sodium sulfate, and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=85:15). The purified product was condensed under reduced pressure, and the residue was recrystallized from ether/hexane, thereby obtaining the title compound (0.18 g) as a pale brownish white powder.

Quelle