Reacción #90072

Ecuación de reacción

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

Disolventes

NMP

ethyl acetate

Condiciones de reacción

Tratamiento posterior

1. 1
   Lavadowashed with water
2. 2
   Secadodried over magnesium sulfate
3. 3
   OtroThe drying agent was removed by filtration
4. 4
   Otrothe residues obtained
5. 5
   Concentraciónafter concentration under reduced pressure
6. 6
   Otrowere purified by silica gel column chromatography (hexane/ethyl acetate)
7. 7
   Otroto obtain the target compound (white solid, 101 mg, 3%)

Procedimiento

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%).

Fuente