Reacción #2063059

Ecuación de reacción

1-(4-bromophenyl)piperazine

ethyl (2-chloroethyl)-carbamate

Triethylamine

→

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

Rendimiento 67.2%

Disolventes

CH2Cl2

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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).

Fuente