N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine → N-[(6-chloropyridin-3-yl)methyl]-N-(2,2-difluoroethyl)-4-hydroxy-2-oxo-2,5-dihydrofuran-3-carboxamide

HRID 1192839

Reaktionsgleichung

[OH:1][C:2]1[CH2:6][O:5][C:4](=[O:7])[C:3]=1[C:8]([O:10]C)=O.[Cl:12][C:13]1[N:18]=[CH:17][C:16]([CH2:19][NH:20][CH2:21][CH:22]([F:24])[F:23])=[CH:15][CH:14]=1>C(#N)CCC>[Cl:12][C:13]1[N:18]=[CH:17][C:16]([CH2:19][N:20]([CH2:21][CH:22]([F:24])[F:23])[C:8]([C:3]2[C:4](=[O:7])[O:5][CH2:6][C:2]=2[OH:1])=[O:10])=[CH:15][CH:14]=1

Komponenten

Reaktionsbedingungen

Temperatur: 65 °C

Versuchsvorschrift

10 g of methyl 4-hydroxy-2-oxo-2,5-dihydrofuran-3-carboxylate are initially introduced in 111 g of butyronitrile and admixed with 5 g of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine. The solution is heated at 65° C. for 3 h. The solution is then extracted with 300 ml of water and then washed with 300 ml of 5% strength hydrochloric acid solution. The organic phase is dried over magnesium sulphate and the solvent is removed in vacuo. For purification, recrystallization from isopropanol is carried out.

Aufarbeitung

extractionThe solution is then extracted with 300 ml of water
washwashed with 300 ml of 5% strength hydrochloric acid solution
dry with materialThe organic phase is dried over magnesium sulphate
customthe solvent is removed in vacuo
customFor purification, recrystallization from isopropanol

Quellen und Nachweise

ORD-Eintrag: ord-33b2f7e565e44cbd870ad14183a7eeae
Quelldatensatz: uspto-grants-2014_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08680285B2

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