Reaktion #2456405

Reaktionsgleichung

2-indanone

phenyl hydrazine

→

5,10-dihydroindeno[1,2-b]indole

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution was warmed
2. 2
   Sonstigewas removed from the oil bath
3. 3
   Temperaturto cool to room temperature
4. 4
   SonstigeLight yellow needle-like crystals precipitated from the solution
5. 5
   TemperaturUpon cooling to room temperature
6. 6
   Temperaturthe solution was cooled to 0° C. for 30 minutes
7. 7
   FiltrationThe crystals were filtered via vacuum filtration
8. 8
   Sonstigeused without further purification

Vorschrift

A modified version of the method reported by Okamoto, et al. was employed. Okamoto, T. A.; Kobayashi, S. M.; Yamamoto, H. N., DE1952019, 1970. To a solution of 2-indanone (16.3 g, 123 mmol) in ethanol (80 mL) was added phenyl hydrazine (12.1 mL, 123 mmol) followed by acetic acid (12 drops) at room temperature. While stirring, the solution was warmed to reflux (oil bath at 85° C.) for 15 minutes at which point it was removed from the oil bath and allowed to cool to room temperature. Light yellow needle-like crystals precipitated from the solution. Upon cooling to room temperature, the solution was cooled to 0° C. for 30 minutes. The crystals were filtered via vacuum filtration and used without further purification.

Quelle