Reaktion #2063064

Reaktionsgleichung

1-(3,4-dichlorophenyl)-piperazine

1-bromo-2-chloroethane

triethylamine

→

4-(2-chloroethyl)-1-(3,4-dichlorophenyl)-piperazine

Ausbeute 35.4%

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was cooled
2. 2
   Sonstigepartitioned between CH2Cl2 and water
3. 3
   SonstigeThe layers were separated
4. 4
   FiltrationThe organic phase was filtered over dicalite
5. 5
   SonstigeThe organic filtrate was dried
6. 6
   Filtrationfiltered
7. 7
   Sonstigethe filtrate was evaporated
8. 8
   SonstigeThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2)
9. 9
   SonstigeThe pure fractions were collected
10. 10
    Sonstigethe solvent was evaporated

Vorschrift

A mixture of 1-(3,4-dichlorophenyl)-piperazine (0.05 mol), 1-bromo-2-chloroethane (0.1 mol) and triethylamine (0.05 mol) was stirred for 30 minutes at 100° C. The mixture was cooled, then partitioned between CH2Cl2 and water. The layers were separated. The organic phase was filtered over dicalite. The organic filtrate was dried, filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2). The pure fractions were collected and the solvent was evaporated, yielding 5.2 g (35%) of 4-(2-chloroethyl)-1-(3,4-dichlorophenyl)-piperazine (interm. 9).

Quelle