Sodium Chloride → HCID 67261521, Verbindung

Reaktionsgleichung

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

Komponenten

Reaktionsbedingungen

Temperatur: 95 °C

Versuchsvorschrift

A mixture of 7-chloro-N-(3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-yl)imidazo[1,2-a]pyridine-3-carboxamide (1.0 g, 2.2 mmol; prepared as in Example 65, step C)), 2-(2-(vinyloxy)ethoxy)ethanol (1.2 g, 8.8 mmol) and potassium hydroxide (0.61 g, 11 mmol) was dissolved in DMSO (10 mL). The reaction mixture was heated at 95° C. for 20 hours. The mixture was cooled to ambient temperature, transferred into water (100 mL) and saturated aqueous NaCl (200 mL) and stirred at ambient temperature for 4 hours. The resulting solid was collected by vacuum filtration and dried under vacuum to give the product (0.90 g). MS (ES+APCI) m/z=552.9 (M+H).

Aufarbeitung

temperatureThe mixture was cooled to ambient temperature
filtrationThe resulting solid was collected by vacuum filtration
customdried under vacuum

Quellen und Nachweise

ORD-Eintrag: ord-b706fceb46114a53b66c3ac276599b52
Quelldatensatz: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08841455B2

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