Reaktion #1569780
ord-57d7bc0cd97047cbbbbae1c320fe17e6
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwere respectively added
- 2workup.ADDITIONmixed
- 3Temperaturheated
- 4Temperaturrefluxed
- 5Sonstigeto react for 15 hours
- 6Filtrationfiltered
- 7EinengenThe filtrate was concentrated
- 8Sonstigeto produce oily products
- 9workup.ADDITIONtreated by chromatography with neutral Al2O3
- 10Sonstigepurified
- 11Wascheneluted with dichloromethane
Vorschrift
1-(4-chlorobutyl)-1H-benzotriazole (7.55 g, 0.036 mol) was dissolved into 100 ml of acetonitrile, 3-cyano phenylpiperazine (5.6 g, 0.03 mol), diisopropylethylamine (15.5 g, 0.12 mol) and potassium iodide (5.0 g, 0.03 mol) were respectively added. The mixture was stirred and mixed, then heated and refluxed to react for 15 hours. The mixture was cooled down to ambient temperature and filtered. The filtrate was concentrated to produce oily products, and treated by chromatography with neutral Al2O3 and purified, eluted with dichloromethane to produce 7.6 g compound (I-41) with a yield of 70.5%. ESI-MS [M+H]+: m/z 360.2.