Reaktion #156169

Reaktionsgleichung

Tributyl phosphine

1,1′-(azodicarbonyl)dipiperidine

2-nitro-N-[2-(1-oxo-1H-isoquinolin-2-yl)-ethyl]-benzenesulfonamide

1-ethyl-7-(3-hydroxy-propyl)-3,3,5-trimethyl-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione

→

title compound

Ausbeute 26.5%

N-[3-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-yl)propyl]-2-nitro-N-[2-(1-oxo-1H-isoquinolin-2-yl)ethyl]benzenesulfonamide

Ausbeute 26.5%

Lösungsmittel

toluene

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionfollowed by extraction
2. 2
   WaschenThe organic layer was washed with water and saturated saline
3. 3
   Trocknendried with magnecium sulfate, and condensed under reduced pressure
4. 4
   SonstigeThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→1:0)
5. 5
   Sonstigecondensed under reduced pressure

Vorschrift

Tributyl phosphine (1.2 ml) and 1,1′-(azodicarbonyl)dipiperidine (1.17 g) were added to a toluene solution (100 ml) of 2-nitro-N-[2-(1-oxo-1H-isoquinolin-2-yl)-ethyl]-benzenesulfonamide (1.39 g), and 1-ethyl-7-(3-hydroxy-propyl)-3,3,5-trimethyl-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione (0.94 g). The mixture was stirred overnight. Water was added to the reaction mixture, followed by extraction using ethyl acetate. The organic layer was washed with water and saturated saline, dried with magnecium sulfate, and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:1→1:0). The purified product was condensed under reduced pressure to produce the title compound (0.54 g) as a white amorphous.

Quelle