Diisopropyl Ether → HCID 22492950, Verbindung

To a suspension of 1-[4-[5-(4-iodophenyl)-1,3,4-thiadiazol-2-yl]phenyl]-4-(4-methylcyclohexyl)piperazine (2 g) in DMF (40 ml) was successively added ethyl formate (0.56 ml), dichlorobis(triphenylphosphine)palladium(II) (0.52 g) and 20% sodium ethoxide ethanol solution (4.43 ml) with stirring and the mixture was stirred at 40° C. for 2 hours. The reaction mixture was added diisopropyl ether (600 ml). The resulting precipitate was collected by filtration. The precipitate was dissolved THF (200 ml), insoluble materials were filtered off and solution was concentrated in vacuo. The resulting residue was washed with acetonitrile, and dried to give ethyl 4-[5-[4-[4-(4-methylcyclohexyl)-1-piperazinyl]phenyl]-1,3,4-thiadiazol-2-yl]benzoate (1.07 g).

1. stirringthe mixture was stirred at 40° C. for 2 hours
2. filtrationThe resulting precipitate was collected by filtration
3. dissolutionThe precipitate was dissolved THF (200 ml), insoluble materials
4. filtrationwere filtered off
5. concentrationsolution was concentrated in vacuo
6. washThe resulting residue was washed with acetonitrile
7. customdried

ORD-Eintrag

ord-ab64febad9a54cee84fea87e5c031566

Quelldatensatz

uspto-grants-2005_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06884774B2