反应 #1269902

反应方程式

1′-Benzyl-5-fluoro-3H-spiro[2-benzofuran-1,4′-piperidin]-3-one

→

5-fluoro-3H-spiro[2-benzofuran-1,4′-piperidin]-3-one

收率 96.0%

溶剂

ethanol

反应条件

后处理

1. 1
   温度The mixture was refluxed under an hydrogen atmosphere for 1 hour
2. 2
   其他purged with argon
3. 3
   workup.ADDITIONdiluted with dichloromethane
4. 4
   过滤The catalyst was filtered
5. 5
   浓缩the filtrate was concentrated in vacuo
6. 6
   workup.DISSOLUTIONThe white solid was dissolved in water (20 ml)
7. 7
   萃取extracted 3 times with dichloromethane
8. 8
   干燥The combined extracts were dried over Na2SO4
9. 9
   过滤filtered
10. 10
    浓缩concentrated in vacuo

实验过程

1′-Benzyl-5-fluoro-3H-spiro[2-benzofuran-1,4′-piperidin]-3-one (0.622 g, 2 mmol) was suspended in ethanol (6 ml). The mixture was acidified with a few drops of HCl 37%. Pd/C 10% (65 mg, 0.06 mmol) was added. The mixture was refluxed under an hydrogen atmosphere for 1 hour then cooled to room temperature, purged with argon and diluted with dichloromethane. The catalyst was filtered and the filtrate was concentrated in vacuo. The white solid was dissolved in water (20 ml). The solution was basified with a 2M Na2CO3 solution and extracted 3 times with dichloromethane. The combined extracts were dried over Na2SO4, filtered and concentrated in vacuo to yield 0.42 g (96%) 5-fluoro-3H-spiro[2-benzofuran-1,4′-piperidin]-3-one as a white solid. MS m/e: 222 (M+H+).

来源