تفاعل #2063064

معادلة التفاعل

1-(3,4-dichlorophenyl)-piperazine

1-bromo-2-chloroethane

triethylamine

→

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

المردود 35.4%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was cooled
2. 2
   أخرىpartitioned between CH2Cl2 and water
3. 3
   أخرىThe layers were separated
4. 4
   ترشيحThe organic phase was filtered over dicalite
5. 5
   أخرىThe organic filtrate was dried
6. 6
   ترشيحfiltered
7. 7
   أخرىthe filtrate was evaporated
8. 8
   أخرىThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2)
9. 9
   أخرىThe pure fractions were collected
10. 10
    أخرىthe solvent was evaporated

الإجراء التجريبي

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).

المصدر