반응 #2063061
ord-3cd5094adeef4f49b75cd011c0efecde
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도refluxed for one hour
- 2기타The solvent was evaporated
- 3기타the residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
- 4기타The pure fractions were collected
- 5기타the solvent was evaporated
- 6workup.STIRRINGThe residue was stirred in diisopropylether/acetonitrile 10/1
- 7기타The solvent was evaporated
실험 절차
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).