反応 #2063059

反応方程式

1-(4-bromophenyl)piperazine

ethyl (2-chloroethyl)-carbamate

Triethylamine

→

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

収率 67.2%

溶媒

CH2Cl2

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred for 15 minutes at 130° C
2. 2
   温度The reaction mixture was cooled to room temperature
3. 3
   洗浄the resulting mixture was washed with water
4. 4
   その他The organic layer was separated
5. 5
   その他dried
6. 6
   ろ過filtered
7. 7
   その他the solvent was evaporated
8. 8
   その他The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
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-(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).

出典