Water → Methyl 6-{3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)-pyrrolidin-1-yl}-4-(trifluoromethyl)nicotinate

HRID 2206914

Reaktionsgleichung

Cl[C:2]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=1.[F:16][C:17]([F:38])([F:37])[C:18]1[CH:19]=[C:20]([C:28]2([C:33]([F:36])([F:35])[F:34])[CH2:32][CH2:31][NH:30][CH2:29]2)[CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O.C(OCC)(=O)C>[F:26][C:24]([F:25])([F:27])[C:22]1[CH:21]=[C:20]([C:28]2([C:33]([F:36])([F:34])[F:35])[CH2:32][CH2:31][N:30]([C:2]3[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=3)[CH2:29]2)[CH:19]=[C:18]([C:17]([F:16])([F:37])[F:38])[CH:23]=1

Komponenten

Reaktionsbedingungen

Temperatur: 80 °C

Versuchsvorschrift

Methyl 6-chloro-4-(trifluoromethyl)nicotinate (2.39 g), 3-[3,5-bis(trifluoromethyl)-phenyl]-3-(tri-fluoromethyl)pyrrolidine (2.98 g) and potassium carbonate (1.8 g) were suspended in dimethylformamide (50 ml). The reaction mixture was heated for 8 hours at 80° C. Water and ethyl acetate were added and the extraction was carried out. The extract was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The target compound (3.07 g) was obtained by purification with silica gel column chromatography.

Aufarbeitung

extractionthe extraction
dry with materialThe extract was dried over magnesium sulfate
filtrationfiltered
concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-290fb8e9b01e422cb99952c9f972d628
Quelldatensatz: uspto-grants-2016_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09375000B2

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