Water → HCID 72189950, Verbindung

HRID 705712Notizen

Reaktionsgleichung

[Cl:1][C:2]1[C:7]2OCO[C:6]=2[CH:5]=[C:4]([C:11]2[C:15]([C:16]([F:19])([F:18])[F:17])=[N:14][N:13]([C:20]3[N:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[C:12]=2[NH2:26])[CH:3]=1.[H-].[Na+].[CH2:29]([N:31]=[C:32]=[O:33])[CH3:30].[OH2:34]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([C:11]2[C:15]([C:16]([F:18])([F:17])[F:19])=[N:14][N:13]([C:20]3[N:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[C:12]=2[N:26]([C:32](=[O:33])[NH:31][CH2:29][CH3:30])[C:20]([NH:13][CH2:12][CH3:11])=[O:34])[CH:5]=[C:6]([C:16]([F:19])([F:18])[F:17])[CH:7]=1

Komponenten

Reaktionsbedingungen

Temperatur: 22.5 °C

Versuchsvorschrift

To a mixture of 4-(7-chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine (0.200 g, 0.50 mmol) and NaH (0.015 g, 0.64 mmol) in tetrahydrofurane is added ethylisocyanate (0.078 g, 1.10 mmol). The mixture is refluxed for 4 hours. The reaction was cooled to room temperature (20-25° C.), diluted with water and extracted with ethyl acetate; the organic layer separated and further washed with water and then dried and concentrated. The residue was re-crystallized with a mixture of ethyl acetate and petrole ether to give the title compound (46 mg; 16%).

Aufarbeitung

temperatureThe mixture is refluxed for 4 hours
extractionextracted with ethyl acetate
customthe organic layer separated
washfurther washed with water
customdried
concentrationconcentrated
customThe residue was re-crystallized with a mixture of ethyl acetate and petrole ether

Quellen und Nachweise

ORD-Eintrag: ord-b7c683e1709b4d04807de170b618379b
Quelldatensatz: uspto-grants-2015_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09174967B2

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