反应 #2063059

反应方程式

1-(4-bromophenyl)piperazine

ethyl (2-chloroethyl)-carbamate

Triethylamine

→

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

收率 67.2%

溶剂

CH2Cl2

反应条件

后处理

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
   洗涤the resulting mixture was washed with water
4. 4
   其他The organic layer was separated
5. 5
   其他dried
6. 6
   过滤filtered
7. 7
   其他the solvent was evaporated
8. 8
   其他The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
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-(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).

来源