Reaktion #84533

Reaktionsgleichung

N-(3-fluoro-4-morpholinophenyl)-3-oxobutanamide

Br2

→

title compound

Ausbeute 47.0%

4-bromo-N-(3-fluoro-4-morpholinophenyl)-3-oxobutanamide

Ausbeute 47.0%

Lösungsmittel

AcOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAt end of addition
2. 2
   EinengenThe mixture was then concentrated in vacuo and 40 mL of water
3. 3
   workup.ADDITIONwas added
4. 4
   ExtraktionThe resulting mixture was extracted with EtOAc (30 mL×4)
5. 5
   WaschenThe combined organic phases were washed with brine (40 mL×3)
6. 6
   Trocknendried over anhydrous Na2SO4
7. 7
   Einengenconcentrated in vacuo
8. 8
   SonstigeThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1)

Vorschrift

To a solution of N-(3-fluoro-4-morpholinophenyl)-3-oxobutanamide (11.2 g, 40.0 mmol) and AcOH (100 mL) under N2 was added Br2 (2.4 mL) at rt. At end of addition, the mixture was stirred further at rt for 24 h. The mixture was then concentrated in vacuo and 40 mL of water was added. The resulting mixture was extracted with EtOAc (30 mL×4). The combined organic phases were washed with brine (40 mL×3), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1) to give the title compound as a yellow solid (6.80 g, 47%).

Quelle