반응 #75608

반응 방정식

1-benzyl-4-piperidine carboxamide

phosphorus oxychloride

→

1-benzyl-4-piperidine carbonitrile

수율 94.4%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타It was evaporated
3. 3
   workup.DISSOLUTIONthe resulting residue was dissolved in ethyl acetate
4. 4
   세척washed with aqueous sodium hydroxide and brine
5. 5
   건조After drying over anhydrous sodium sulfate, it
6. 6
   기타was evaporated
7. 7
   기타the resulting residue was purified by silica gel column chromatography

실험 절차

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.

출처