Cesium carbonate → HCID 58043775, Verbindung
Reaktionsgleichung
[C:1]12[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:8][C:7]1[C:6](=[O:14])[NH:5][CH2:4][CH2:3][C:2]2=1.[C:15]([O:18][CH2:19][C:20]1[C:25]([Br:26])=[CH:24][C:23]([F:27])=[CH:22][C:21]=1Br)(=[O:17])[CH3:16].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.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]>[C:15]([O:18][CH2:19][C:20]1[C:21]([N:5]2[C:6](=[O:14])[C:7]3[S:8][C:9]4[CH:10]=[CH:11][CH:12]=[CH:13][C:1]=4[C:2]=3[CH2:3][CH2:4]2)=[CH:22][C:23]([F:27])=[CH:24][C:25]=1[Br:26])(=[O:17])[CH3:16]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
A mixture of 329f (700 mg, 3.4 mmol), 197c (3.35 g, 10.2 mmol), XantPhos (200 mg, 0.34 mmol), Pd2(dba)3 (316 mg, 0.34 mmol) and Cs2CO3 (2.25 g, 6.8 mmol) in dioxane (50 mL) was heated at 100° C. for 15 h under argon atmosphere. It was then filtered and evaporated in vacuo. The residue was purified by column chromatography eluting with 1:3 ethyl acetate/petroleum ether to give 329g as a white solid (500 mg, 33%). MS: [M+H]+ 448.
Aufarbeitung
- filtrationIt was then filtered
- customevaporated in vacuo
- customThe residue was purified by column chromatography
- washeluting with 1:3 ethyl acetate/petroleum ether
Quellen und Nachweise
- ORD-Eintrag
- ord-fb2a9b57dbf84fb0adb5360fff733726
- Quelldatensatz
- uspto-grants-2013_12
- Patentnummer
- US08618107B2
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