Methylhydrazine → HCID 67548813, Verbindung
Reaktionsgleichung
F[C:2]1[C:7]([CH:8]=O)=[C:6]([I:10])[CH:5]=[CH:4][N:3]=1.[CH3:11][NH:12][NH2:13]>>[I:10][C:6]1[CH:5]=[CH:4][N:3]=[C:2]2[N:12]([CH3:11])[N:13]=[CH:8][C:7]=12Komponenten
3
Versuchsvorschrift
227 mg of 2-fluoro-4-iodo-pyridine-3-carbaldehyde (0.9 mmol, 1 eq.; prepared as described in J. Org. Chem. 1993, 58, 7832) were dissolved in 3.6 mL 1-PrOH, treated with 72 μL methyl hydrazine (1.36 mmol, 1.5 eq.) and heated to 100° C. for 30 min (Biotage Initiator 60®). The reaction mixture was concentrated in vacuo, the residue was partioned between water and ethyl acetate, the aq. layer was extracted with ethyl acetate, the combined organic layers were dried and concentrated in vacuo to provide the crude target compound.
Aufarbeitung
- concentrationThe reaction mixture was concentrated in vacuo
- extractionthe aq. layer was extracted with ethyl acetate
- customthe combined organic layers were dried
- concentrationconcentrated in vacuo
- customto provide the crude target compound
Quellen und Nachweise
- ORD-Eintrag
- ord-48cca360379648a7a0de081b6ed67cb3
- Quelldatensatz
- uspto-grants-2010_12
- Patentnummer
- US07846928B2
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