تفاعل #2063059

معادلة التفاعل

1-(4-bromophenyl)piperazine

ethyl (2-chloroethyl)-carbamate

Triethylamine

→

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

المردود 67.2%

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر