Reaktion #74908

Reaktionsgleichung

5-chloro-1-indanone

nitric acid

→

5-Chloro-6-nitro-1-indanone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeremains between -10° and -15° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   workup.ADDITIONthe reaction solution is poured onto ice
4. 4
   Sonstigethe precipitate which has separated out
5. 5
   Filtrationis filtered off
6. 6
   Waschenwashed with water
7. 7
   SonstigeThe crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone
8. 8
   Sonstigerises to 126°-128° C.

Vorschrift

86.0 g (0.51 mole) of 5-chloro-1-indanone are introduced in portions into 540 ml of fuming nitric acid (d=1.54), cooled to -20° C., so that the temperature of the reaction mixture remains between -10° and -15° C. After the addition has ended, the mixture is subsequently stirred for 45 minutes at -15° to -20° C., the reaction solution is poured onto ice and the precipitate which has separated out is filtered off and washed with water. The crude product of melting point 110°-113° is recrystallized from ethanol, whereby the melting point of the pure 5-chloro-6-nitro-1-indanone rises to 126°-128° C.

Quelle