Potassium Phosphate, Tribasic → HCID 23157344, Verbindung

HRID 507978Notizen

Reaktionsgleichung

FC(F)(F)S(O[C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH2:9][CH2:10][C:11]2=[O:16])(=O)=O.[CH3:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=1B(O)O.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2)CCCCC1.C1(C)C=CC=CC=1>[CH3:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=1[C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH2:9][CH2:10][C:11]2=[O:16]

Komponenten

Reaktionsbedingungen

Temperatur: 90 °C

Versuchsvorschrift

A mixture of 1-oxo-2,3-dihydro-1H-inden-4-yl trifluoromethanesulfonate (10.0 g, 35.7 mmol), 2,6-dimethylphenylboronic acid (6.96 g, 46.4 mmol), 2-(dicyclohexylphosphino)biphenyl (750 mg, 2.14 mmol), tris(dibenzylideneacetone)dipalladium(0) (1.31 mg, 1.43 mmol), tripotassium phosphate (15.2 g, 71.4 mmol) and toluene (200 mL) was heated under reflux under an argon atmosphere at 90° C. for 16 hr. After cooling the reaction mixture, the insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5%-45% ethyl acetate/hexane) to give the title compound (7.21 g, yield 85%) as pale-yellow crystals.

Aufarbeitung

temperaturewas heated
temperatureAfter cooling the reaction mixture
filtrationthe insoluble material was filtered off
concentrationthe filtrate was concentrated under reduced pressure
customThe residue was purified by silica gel column chromatography (5%-45% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag: ord-abf8d35e7cc94dea9775d44c982f1409
Quelldatensatz: uspto-grants-2010_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07786165B2

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