Reaktion #86186

Reaktionsgleichung

6-bromo-2-fluoro-3-methoxy-pyridine

1,4-diazepan-6-ol dihydrobromide

N,N′-diisopropylethylamine

→

1-(6-bromo-3-methoxy-2-pyridyl)-1,4-diazepan-6-ol

Ausbeute 37.5%

Lösungsmittel

Isopropanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was cooled to room temperature
2. 2
   Einengenconcentrated
3. 3
   SonstigeThe residue was purified on silica
4. 4
   Wascheneluted with 0 to 10% MeOH in DCM

Vorschrift

A mixture of 6-bromo-2-fluoro-3-methoxy-pyridine (2.660 mmol; 547.9 mg), 1,4-diazepan-6-ol dihydrobromide (3.989 mmol; 1109 mg), and N,N′-diisopropylethylamine (10.64 mmol; 1389 mg; 1.87 mL) in Isopropanol (10 mL) in a sealed pressure vial was heated at 100° C. overnight. The mixture was cooled to room temperature and concentrated. The residue was purified on silica eluted with 0 to 10% MeOH in DCM to afford 1-(6-bromo-3-methoxy-2-pyridyl)-1,4-diazepan-6-ol (301.2 mg, 37%).

Quelle