Reaktionsgleichung
[C:1]1([N:7]=[N+]=[N-])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(P(C2C=CC=CC=2)CCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C[Mg]Br.C1C[O:44][CH2:43][CH2:42]1>>[C:43]([NH:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:44])[CH3:42]Komponenten
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
In a capped vial (1 mL) containing a solution of phenylazide (6.6 mg, 55 μmol) in dry THF (300 μL), was added [RhCl(cod)]2 (0.27 mg, 0.55 μmol), and 1,2-bis(diphenylphosphino)ethane (0.66 mg, 1.65 μmol), and was shaken until the solution was homogeneous. After addition of a solution of methyl magnesium bromide (18.5 μL of 3M solution in ether, 55 μmol), the resulting mixture was transferred to the micro-autoclave, which was pre-charged with [11C]CO. The micro-autoclave was heated at 120° C. for 5 min under 35 MPa and the crude product was transferred to a reduced pressure vial. The radioactivity was measured before and after the vial was flushed with N2 (the [11C]CO-trapping efficiency of 96% was determined based on these values). The solution was dissolved in ammonium formate (0.5 mL, pH=3.5) and heated at 120° C. for 1 min. A small amount of crude product was collected and analyzed by the reversed phase HPLC. Yield of product: 91%. The product was identified by HPLC with an added authentic reference compound.
Aufarbeitung
- additionwas pre-charged with [11C]CO
- customwas flushed with N2 (the [11C]CO-
- dissolutionThe solution was dissolved in ammonium formate (0.5 mL, pH=3.5)
- temperatureheated at 120° C. for 1 min
- customA small amount of crude product was collected
Quellen und Nachweise
- ORD-Eintrag
- ord-762bd504a5d649efb367b630688e8be4
- Quelldatensatz
- uspto-grants-2014_06
- Patentnummer
- US08741261B2
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