Reaktion #1587725

Reaktionsgleichung

4-Chlorobenzo[b]thiophene

piperazine

tri-tert-butylphosphonium tetraphenylborate

sodium tert-butoxide

→

4-(1-piperazinyl)benzo[b]thiophene hydrochloride

Lösungsmittel

water

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe layers were separated
2. 2
   WaschenThe xylene layer was washed with water
3. 3
   workup.ADDITIONAfter addition of activated carbon
4. 4
   FiltrationAfter filtration of the mixture, concentrated hydrochloric acid
5. 5
   workup.ADDITIONwas added to the filtrate
6. 6
   workup.STIRRINGthe resulting mixture was stirred at room temperature for 30 minutes
7. 7
   FiltrationThe precipitated crystals were collected by filtration
8. 8
   Sonstigedried

Vorschrift

4-Chlorobenzo[b]thiophene (5.00 g), piperazine (5.11 g), palladium acetate (II) (2.7 mg), tri-tert-butylphosphonium tetraphenylborate (6.2 mg), sodium tert-butoxide (8.548 g), and xylene (70 ml) were stirred at 120 to 130° C. for 5 hours. After the reaction mixture was cooled to room temperature, water was added thereto, and the layers were separated. The xylene layer was washed with water, and then with saline. After addition of activated carbon, the mixture was stirred at room temperature for 30 minutes. After filtration of the mixture, concentrated hydrochloric acid was added to the filtrate, and the resulting mixture was stirred at room temperature for 30 minutes. The precipitated crystals were collected by filtration and dried to obtain 4-(1-piperazinyl)benzo[b]thiophene hydrochloride.

Quelle