تفاعل #1269902

معادلة التفاعل

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

→

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

المردود 96.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was refluxed under an hydrogen atmosphere for 1 hour
2. 2
   أخرىpurged with argon
3. 3
   workup.ADDITIONdiluted with dichloromethane
4. 4
   ترشيحThe catalyst was filtered
5. 5
   تركيزthe filtrate was concentrated in vacuo
6. 6
   workup.DISSOLUTIONThe white solid was dissolved in water (20 ml)
7. 7
   استخلاصextracted 3 times with dichloromethane
8. 8
   تجفيفThe combined extracts were dried over Na2SO4
9. 9
   ترشيحfiltered
10. 10
    تركيزconcentrated in vacuo

الإجراء التجريبي

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+).

المصدر