反应 #2063064

反应方程式

1-(3,4-dichlorophenyl)-piperazine

1-bromo-2-chloroethane

triethylamine

→

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

收率 35.4%

反应条件

后处理

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

实验过程

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).

来源