Reaktion #90072

Reaktionsgleichung

2-Hydrazinopyridine

7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one

7-Methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one

Compound A2

7-Methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one

→

8-Methoxy-10,10-dimethyl-10,11-dihydro-5H-1,11-diaza-benzo[B]fluorene

Lösungsmittel

NMP

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with water
2. 2
   Trocknendried over magnesium sulfate
3. 3
   SonstigeThe drying agent was removed by filtration
4. 4
   Sonstigethe residues obtained
5. 5
   Einengenafter concentration under reduced pressure
6. 6
   Sonstigewere purified by silica gel column chromatography (hexane/ethyl acetate)
7. 7
   Sonstigeto obtain the target compound (white solid, 101 mg, 3%)

Vorschrift

2-Hydrazinopyridine (1.3 g, 11.8 mmol) and 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 2.4 g, 11.8 mmol) were dissolved in NMP (60 mL), and stirred at 190° C. for 48 hr. The reaction solution was diluted with ethyl acetate, washed with water and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the target compound (white solid, 101 mg, 3%).

Quelle