反応 #2063061

反応方程式

1-(3,4-dichlorophenyl)piperazine

2-propenenitrile

→

4-(3,4-dichlorophenyl)-1-piperazinepropanenitrile

収率 98.5%

溶媒

2-propanol

反応条件

後処理

1. 1
   温度refluxed for one hour
2. 2
   その他The solvent was evaporated
3. 3
   その他the residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
4. 4
   その他The pure fractions were collected
5. 5
   その他the solvent was evaporated
6. 6
   workup.STIRRINGThe residue was stirred in diisopropylether/acetonitrile 10/1
7. 7
   その他The solvent was evaporated

実験手順

A mixture of 1-(3,4-dichlorophenyl)piperazine (0.1 mol), 2-propenenitrile (0.15 mol), and N-methyl-N,N-dioctyl octanaminiumchloride (1 ml) in 2-propanol (150 ml) was stirred and refluxed for one hour. The solvent was evaporated and 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. The residue was stirred in diisopropylether/acetonitrile 10/1. The solvent was evaporated, yielding 28 g (98.5%) of 4-(3,4-dichlorophenyl)-1-piperazinepropanenitrile (intern. 3).

出典