反応 #2063064

反応方程式

1-(3,4-dichlorophenyl)-piperazine

1-bromo-2-chloroethane

triethylamine

→

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

収率 35.4%

反応条件

後処理

1. 1
   温度The mixture was cooled
2. 2
   その他partitioned between CH2Cl2 and water
3. 3
   その他The layers were separated
4. 4
   ろ過The organic phase was filtered over dicalite
5. 5
   その他The organic filtrate was dried
6. 6
   ろ過filtered
7. 7
   その他the filtrate was evaporated
8. 8
   その他The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2)
9. 9
   その他The pure fractions were collected
10. 10
    その他the solvent was evaporated

実験手順

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).

出典