Sodium Carbonate → HCID 131732832, Verbindung

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Reaktionsgleichung

Br[C:2]1[C:6]2=[N:7][CH:8]=[CH:9][CH:10]=[C:5]2[N:4]([CH2:11][CH3:12])[N:3]=1.CC1(C)C(C)(C)OB([C:21]2[CH:26]=[CH:25][C:24]([C:27]([C:34]3[N:38]([CH2:39][O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])[C:37]4[CH:47]=[CH:48][CH:49]=[CH:50][C:36]=4[N:35]=3)=[CH:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:23][CH:22]=2)O1.C([O-])([O-])=O.[Na+].[Na+]>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1COCC1>[CH2:11]([N:4]1[C:5]2[C:6](=[N:7][CH:8]=[CH:9][CH:10]=2)[C:2]([C:21]2[CH:26]=[CH:25][C:24]([C:27]([C:34]3[N:38]([CH2:39][O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])[C:37]4[CH:47]=[CH:48][CH:49]=[CH:50][C:36]=4[N:35]=3)=[CH:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:23][CH:22]=2)=[N:3]1)[CH3:12]

Komponenten

Reaktionsbedingungen

Temperatur: 150 °C

Versuchsvorschrift

A mixture of 3-bromo-1-ethyl-1H-pyrazolo[4,3-b]pyridine (300 mg), ethyl 3-{4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl}-3-(1-[{2-(trimethylsilyl)ethoxy}methyl]-1H-benzo[d]imidazol-2-yl)acrylate (1456 mg), Pd(PPh3)4 (77 mg), 2 M Na2CO3 aqueous solution (1.991 mL) and THF (4 mL) was heated at 150° C. for 30 min under microwave irradiation. The reaction mixture was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/AcOEt) to give the title compound (670 mg).

Aufarbeitung

concentrationThe reaction mixture was concentrated under reduced pressure
customThe residue was purified by silica gel column chromatography (hexane/AcOEt)

Quellen und Nachweise

ORD-Eintrag: ord-71753e05df71468191b5e4aacac8730b
Quelldatensatz: uspto-grants-2015_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09029536B2

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