Reaktion #86175

Reaktionsgleichung

2-bromo-6-fluoropyridine

1,4-diazepan-6-ol

DIPEA

→

1-(6-bromopyridin-2-yl)-1,4-diazepan-6-ol

Ausbeute 54.4%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter it was cooled
2. 2
   Einengenthe reaction mixture was concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with EtOAc (100 mL)
4. 4
   Waschenwashed with brine
5. 5
   TrocknenThe organic layer was dried over Na2SO4
6. 6
   Einengenconcentrated under reduced pressure

Vorschrift

A mixture of 2-bromo-6-fluoropyridine (477 mg, 2.7 mmol), 1,4-diazepan-6-ol (350 mg, 3 mmol), and DIPEA (1.94 g, 15 mmol) in ethanol (10 mL) was heated at 100° C. for 16 hours. After it was cooled, the reaction mixture was concentrated under reduced pressure. The residue was diluted with EtOAc (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford 1-(6-bromopyridin-2-yl)-1,4-diazepan-6-ol as a colorless oil (400 mg, 48.9%). MS (ESI) m/z: 272 [M+H]+.

Quelle