Water → HCID 16666575, Verbindung

HRID 1511819

Reaktionsgleichung

Cl[C:2]1[N:7]=[C:6]2[N:8]=[C:9]([NH:12][C:13]([NH:15][CH2:16][CH3:17])=[O:14])[CH:10]=[CH:11][C:5]2=[N:4][CH:3]=1.[CH:18]1([CH:24]=[CH:25]B(O)O)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[Na+].[Na+].O>CN(C)C=O.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[CH:18]1(/[CH:24]=[CH:25]/[C:2]2[N:7]=[C:6]3[N:8]=[C:9]([NH:12][C:13]([NH:15][CH2:16][CH3:17])=[O:14])[CH:10]=[CH:11][C:5]3=[N:4][CH:3]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1

Komponenten

Reaktionsbedingungen

Temperatur: 90 °C

Versuchsvorschrift

99.6 mg of 1-(3-chloropyrido[2,3-b]pyrazin-6-yl)-3-ethylurea (0.40 mmol), 73.6 mg of cyclohexylvinylboronic acid (0.48 mmol), 84.4 mg of sodium carbonate (0.80 mmol) and 33.4 mg of [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.04 mmol) were initially charged in 6 ml of dimethylformamide/water (1:1) under nitrogen. The mixture was then heated to 90° C. for 6.5 h. Distilled water was then added to the reaction mixture and the resulting precipitate was filtered off with suction. The further purification was effected by column chromatography on silica gel (ethyl acetate/heptane eluent mixture). A light brown solid was obtained.

Aufarbeitung

filtrationthe resulting precipitate was filtered off with suction
customThe further purification
customA light brown solid was obtained

Quellen und Nachweise

ORD-Eintrag: ord-bb836e82f9204d52b9a74b7116952c80
Quelldatensatz: uspto-grants-2012_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08217042B2

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