Reaktion #86121

Reaktionsgleichung

2-bromo-6-fluoropyridine

tert-butyl 1,4-diazepane-1-carboxylate

DIPEA

→

tert-butyl 4-(6-bromopyridin-2-yl)-1,4-diazepane-1-carboxylate

Ausbeute 50.1%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONthe residue was diluted with EtOAc (100 mL)
3. 3
   WaschenThe solution was washed with brine
4. 4
   Trocknendried over Na2SO4
5. 5
   Einengenconcentrated under reduced pressure

Vorschrift

A mixture of 2-bromo-6-fluoropyridine (500 mg, 2.8 mmol), tert-butyl 1,4-diazepane-1-carboxylate (568 mg, 2.8 mmol) in DIPEA (1.83 g, 14.2 mmol) in ethanol (10 mL) was heated at 100° C. for 16 hours. The reaction mixture was concentrated under reduced pressure and the residue was diluted with EtOAc (100 mL). The solution was washed with brine, dried over Na2SO4, and concentrated under reduced pressure to afford tert-butyl 4-(6-bromopyridin-2-yl)-1,4-diazepane-1-carboxylate as a colorless oil (500 mg, 50%). MS (ESI) m/z: 356 [M+H]+.

Quelle