반응 #84533

반응 방정식

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

Br2

→

title compound

수율 47.0%

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

수율 47.0%

용매

AcOH

반응 조건

후처리

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

실험 절차

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%).

출처