Reaktion #2063059

Reaktionsgleichung

1-(4-bromophenyl)piperazine

ethyl (2-chloroethyl)-carbamate

Triethylamine

→

ethyl [2-[4-(4-bromophenyl)-1-piperazinyl]-ethyl]carbamate

Ausbeute 67.2%

Lösungsmittel

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred for 15 minutes at 130° C
2. 2
   TemperaturThe reaction mixture was cooled to room temperature
3. 3
   Waschenthe resulting mixture was washed with water
4. 4
   SonstigeThe organic layer was separated
5. 5
   Sonstigedried
6. 6
   Filtrationfiltered
7. 7
   Sonstigethe solvent was evaporated
8. 8
   SonstigeThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
9. 9
   SonstigeThe pure fractions were collected
10. 10
    Sonstigethe solvent was evaporated

Vorschrift

A mixture of 1-(4-bromophenyl)piperazine (0.018 mol) and ethyl (2-chloroethyl)-carbamate (0.036 mol) was stirred for 2 hours at 130° C. Triethylamine (3 ml) was added and the mixture was stirred for 15 minutes at 130° C. The reaction mixture was cooled to room temperature, CH2Cl2 was added and the resulting mixture was washed with water. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The pure fractions were collected and the solvent was evaporated, yielding 4.3 g (67.2 %) of ethyl [2-[4-(4-bromophenyl)-1-piperazinyl]-ethyl]carbamate (interm. 1).

Quelle