Methanol → 1-[3-Fluoro-4-(2,2,2-trifluoroacetyl)-phenyl]-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

HRID 80264

Reaktionsgleichung

[F:1][C:2]1[CH:3]=[C:4]([N:14]2[CH2:18][CH2:17][N:16]([C:19]3[CH:20]=[N:21][CH:22]=[CH:23][C:24]=3[CH3:25])[C:15]2=[O:26])[CH:5]=[CH:6][C:7]=1[CH:8]([OH:13])[C:9]([F:12])([F:11])[F:10].CO>C(Cl)Cl.O=[Mn]=O>[F:1][C:2]1[CH:3]=[C:4]([N:14]2[CH2:18][CH2:17][N:16]([C:19]3[CH:20]=[N:21][CH:22]=[CH:23][C:24]=3[CH3:25])[C:15]2=[O:26])[CH:5]=[CH:6][C:7]=1[C:8](=[O:13])[C:9]([F:12])([F:10])[F:11]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

MnO2 (536 mg, 6.165 mmol) was added to 1-[3-fluoro-4-(2,2,2-trifluoro-1-hydroxy-ethyl)-phenyl]-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (I-197a: 325 mg, 0.880 mmol) in DCM (20 mL) under nitrogen atmosphere. The resulting suspension was stirred at 50° C. overnight. The reaction was monitored by TLC (5% MeOH in DCM). The reaction mixture was cooled to room temperature and filtered through celite pad. The filtrate was washed with CHCl3, dried over Na2SO4 and concentrated. The concentrate was washed with hexane and dried to afford 240 mg of the product (74.53% yield).

Aufarbeitung

temperatureThe reaction mixture was cooled to room temperature
filtrationfiltered through celite pad
washThe filtrate was washed with CHCl3
dry with materialdried over Na2SO4
concentrationconcentrated
washThe concentrate was washed with hexane
customdried

Quellen und Nachweise

ORD-Eintrag: ord-671ad7d54fac432a972bf68e36093e81
Quelldatensatz: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: USRE045173E1

Verknüpfte Notizen

Wird geladen…