Reaktionsgleichung
[F:1][C:2]([F:21])([C:7]1[CH:8]=[C:9](OS(C(F)(F)F)(=O)=O)[CH:10]=[CH:11][CH:12]=1)[C:3]([F:6])([F:5])[F:4].[CH:22]([NH:24][C:25](=[O:27])[CH3:26])=[CH2:23].C(N(CC)CC)C.C1(P(C(P(C2C=CC=CC=2)C2C=CC=CC=2)(C)C)C2C=CC=CC=2)C=CC=CC=1>CN(C=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:1][C:2]([F:21])([C:7]1[CH:8]=[C:9]([C:22]([NH:24][C:25](=[O:27])[CH3:26])=[CH2:23])[CH:10]=[CH:11][CH:12]=1)[C:3]([F:6])([F:5])[F:4]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 130 °C
Versuchsvorschrift
To a solution of the crude product of step 1 (0.75 g, 2.2 mmol) in DMF (10 ml) was added N-vinylacetamide (0.37 g, 4.36 mmol), triethylamine (243 mg, 0.33 ml, 2.40 mmol), palladium acetate (20 mg, 4 mol %) and bis(diphenylphosphino)propane (40 mg, 0.1 mmol). The reaction mixture was heated for 30 min at 130° C. using microwaves. The red solution was diluted and washed with hydrochloric acid (1M, 2×15 ml) and sodium hydrogen carbonate (saturated, 20 ml). The organic phase was dried over sodium sulphate and evaporated. Purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane (2:1) gave the desired product.
Aufarbeitung
- additionThe red solution was diluted
- washwashed with hydrochloric acid (1M, 2×15 ml) and sodium hydrogen carbonate (saturated, 20 ml)
- dry with materialThe organic phase was dried over sodium sulphate
- customevaporated
- customPurification of the crude product by silica gel chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-952ca0b47f1a49ef9fa38068bfe476a6
- Quelldatensatz
- uspto-grants-2012_03
- Patentnummer
- US08143242B2
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