Reaktion #156170

Reaktionsgleichung

Lithium hydroxide

thioglycolic acid

DMF

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

→

title compound

Ausbeute 68.3%

1-Ethyl-3,3,5-trimethyl-7-{3-[2-(1-oxo-1H-isoquinolin-2-yl)ethylamino]propyl}-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

Ausbeute 68.3%

Lösungsmittel

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigecondensed under reduced pressure
2. 2
   Extraktionfollowed by extraction
3. 3
   WaschenThe organic layer was washed with water and saturated saline
4. 4
   Trocknendried with magnesium sulfate, and condensed under reduced pressure
5. 5
   SonstigeThe residue was purified by silica gel column chromatography (ethyl acetate:methanol=10:1)
6. 6
   Sonstigecondensed under reduced pressure

Vorschrift

Lithium hydroxide (3.2 g), and thioglycolic acid (2.4 ml) were added to a DMF solution (27.4 ml) of 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 (4.56 g). The mixture was stirred at room temperature for 1 hour. The reaction mixture was condensed under reduced pressure. Water was added to the residue, followed by extraction using dichloromethane. The organic layer was washed with water and saturated saline, dried with magnesium sulfate, and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:methanol=10:1). The purified product was condensed under reduced pressure to produce the title compound (2.24 g) as a yellow oil.

Quelle