반응 #2063059

반응 방정식

1-(4-bromophenyl)piperazine

ethyl (2-chloroethyl)-carbamate

Triethylamine

→

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

수율 67.2%

용매

CH2Cl2

반응 조건

후처리

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

실험 절차

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).

출처