Formic Acid → 5-Bromo-6-fluoro-1H-benzo(d)imidazole
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[C:4]([NH2:10])[C:5]([NH2:9])=[CH:6][C:7]=1[F:8].[CH:11](O)=O>>[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]2[NH:9][CH:11]=[N:10][C:4]=2[CH:3]=1Komponenten
3
Versuchsvorschrift
A mixture of 98 (600 mg, 2.93 mmol) in formic acid (5.0 mL) was heated to reflux overnight. The reaction mixture was concentrated in vacuo to afford a brown oil that was partitioned between EtOAc (300 mL) and a sat'd. aq. NaHCO3 (100 mL). The organic layer was separated, dried (MgSO4), filtered and evaporated in vacuo to afford 550 mg (87%) of 5-bromo-6-fluoro-1H-benzo[d]imidazole (100) as white solid (550 mg, 87%): MS (ESI) m/z=215 [M+1]+.
Aufarbeitung
- temperaturewas heated
- temperatureto reflux overnight
- concentrationThe reaction mixture was concentrated in vacuo
- customto afford a brown oil that
- customwas partitioned between EtOAc (300 mL)
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-82502aacda4948868c5516f8b4e84003
- Quelldatensatz
- uspto-grants-2014_01
- Patentnummer
- US08637537B2
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