Potassium Phosphate, Tribasic → HCID 86637884, Verbindung

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Reaktionsgleichung

Br[C:2]1[N:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[C:11]([C:16]([F:19])([F:18])[F:17])[CH:10]=2)[C:5]([NH2:20])=[C:4]([O:21][C:22]2[CH:27]=[CH:26][C:25]([F:28])=[C:24]([C:29]([F:32])([F:31])[F:30])[CH:23]=2)[N:3]=1.[CH3:33][N:34]([C:36]1[CH:37]=[C:38](B(O)O)[CH:39]=[CH:40][CH:41]=1)[CH3:35].[O-]P([O-])([O-])=O.[K+].[K+].[K+]>C1(C)C=CC=CC=1.C(OCC)C.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]>[CH3:33][N:34]([CH3:35])[C:36]1[CH:41]=[C:40]([C:2]2[N:7]=[C:6]([O:8][C:9]3[CH:14]=[CH:13][C:12]([F:15])=[C:11]([C:16]([F:19])([F:18])[F:17])[CH:10]=3)[C:5]([NH2:20])=[C:4]([O:21][C:22]3[CH:27]=[CH:26][C:25]([F:28])=[C:24]([C:29]([F:32])([F:31])[F:30])[CH:23]=3)[N:3]=2)[CH:39]=[CH:38][CH:37]=1

Komponenten

Reaktionsbedingungen

Temperatur: 75 °C

Versuchsvorschrift

23 g of 2-Bromo-4,6-bis-(4-fluoro-3-trifluoromethyl-phenoxy)-pyrimidin-5-ylamine are dissolved under nitrogen together with 10.7 g of 3-(N,N-dimethylamino)phenylboronic acid, 0.4 g of tris(dibenzylideneacetone)dipalladium, 27.5 g of K3PO4 and 0.7 g of 2-dicyclohexyl-phosphino-2′,6′-dimethoxybiphenyl in 450 ml of toluene. The mixture is heated at 75° C. for 24 h, diluted with diethylether, washed with water and then dried over MgSO4. The solvents are removed under vacuum. 14.8 g of the title compound are isolated as white powder (mp. 110-111° C.) after purification by filtration and recrystallization from cyclohexane.

Aufarbeitung

washwashed with water
dry with materialdried over MgSO4
customThe solvents are removed under vacuum

Quellen und Nachweise

ORD-Eintrag: ord-85135073155747b1be92323ba231afdf
Quelldatensatz: uspto-grants-2013_02
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08367682B2

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