تفاعل #84533

معادلة التفاعل

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

Br2

→

title compound

المردود 47.0%

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

المردود 47.0%

المذيبات

AcOH

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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%).

المصدر