反応 #75608

反応方程式

1-benzyl-4-piperidine carboxamide

phosphorus oxychloride

→

1-benzyl-4-piperidine carbonitrile

収率 94.4%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度cooling
2. 2
   その他It was evaporated
3. 3
   workup.DISSOLUTIONthe resulting residue was dissolved in ethyl acetate
4. 4
   洗浄washed with aqueous sodium hydroxide and brine
5. 5
   乾燥After drying over anhydrous sodium sulfate, it
6. 6
   その他was evaporated
7. 7
   その他the resulting residue was purified by silica gel column chromatography

実験手順

5 ml N,N-dimethylformamide was added to a mixture of 12.7 g 1-benzyl-4-piperidine carboxamide and 60 ml phosphorus oxychloride under ice-cooling, and it was stirred at room temperature for 1.5 hr. It was evaporated, and the resulting residue was dissolved in ethyl acetate and washed with aqueous sodium hydroxide and brine. After drying over anhydrous sodium sulfate, it was evaporated, and the resulting residue was purified by silica gel column chromatography to give 11.0 g of 1-benzyl-4-piperidine carbonitrile.

出典