반응 #2063064

반응 방정식

1-(3,4-dichlorophenyl)-piperazine

1-bromo-2-chloroethane

triethylamine

→

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

수율 35.4%

반응 조건

후처리

1. 1
   온도The mixture was cooled
2. 2
   기타partitioned between CH2Cl2 and water
3. 3
   기타The layers were separated
4. 4
   여과The organic phase was filtered over dicalite
5. 5
   기타The organic filtrate was dried
6. 6
   여과filtered
7. 7
   기타the filtrate was evaporated
8. 8
   기타The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2)
9. 9
   기타The pure fractions were collected
10. 10
    기타the solvent was evaporated

실험 절차

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).

출처