Potassium Carbonate → HCID 53629647, Verbindung

HRID 1011734

Reaktionsgleichung

[CH3:1][C:2]([Si:5]([CH3:30])([CH3:29])[O:6][CH2:7][C@@H:8]([O:10][C:11]1[CH:12]=[C:13]([CH:25]=[C:26]([OH:28])[CH:27]=1)[C:14]([NH:16][C:17]1[CH:21]=[CH:20][N:19]([CH:22]([CH3:24])[CH3:23])[N:18]=1)=[O:15])[CH3:9])([CH3:4])[CH3:3].[N:31]1([C:35]([C:37]2[CH:38]=[C:39]([Cl:44])[C:40](Cl)=[N:41][CH:42]=2)=[O:36])[CH2:34][CH2:33][CH2:32]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[N:31]1([C:35]([C:37]2[CH:38]=[C:39]([Cl:44])[C:40]([O:28][C:26]3[CH:25]=[C:13]([CH:12]=[C:11]([O:10][C@@H:8]([CH3:9])[CH2:7][O:6][Si:5]([C:2]([CH3:4])([CH3:3])[CH3:1])([CH3:30])[CH3:29])[CH:27]=3)[C:14]([NH:16][C:17]3[CH:21]=[CH:20][N:19]([CH:22]([CH3:24])[CH3:23])[N:18]=3)=[O:15])=[N:41][CH:42]=2)=[O:36])[CH2:34][CH2:33][CH2:32]1

Komponenten

Reaktionsbedingungen

Temperatur: 160 °C

Versuchsvorschrift

A solution of 3-[((1S)-2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-1-methylethyl)oxy]-5-hydroxy-N-[1-(1-methylethyl)-1H-pyrazol-3-yl]benzamide (103 mg, 0.24 mmol) and 5-(azetidin-1-ylcarbonyl)-2,3-dichloropyridine (66 mg, 0.29 mmol) in acetonitrile (2 mL), containing potassium carbonate (66 mg, 0.48 mmol), was heated in a microwave reactor at 160° C. for 6 hours. The reaction mixture was filtered and the filtrate evaporated to dryness under reduced pressure and purified by chromatography on silica, eluting with 50-100% ethyl acetate in hexane, to give the required product as a white foam (142 mg).

Aufarbeitung

filtrationThe reaction mixture was filtered
customthe filtrate evaporated to dryness under reduced pressure
custompurified by chromatography on silica
washeluting with 50-100% ethyl acetate in hexane

Quellen und Nachweise

ORD-Eintrag: ord-178e10e597b34bd387e80afe15c878e9
Quelldatensatz: uspto-grants-2011_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07977328B2

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