반응 #74281

반응 방정식

1-benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidine-4-carbonitrile

H2SO4

LAH

→

(1-Benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidin-4-yl)methanamine

수율 85.0%

용매

THF

THF

반응 조건

후처리

1. 1
   기타the resulting reaction mixture
2. 2
   온도was heated to 50° C. for 16 h
3. 3
   기타The reaction was quenched with THF/H2O solution
4. 4
   여과filtered
5. 5
   세척the solid residue washed with excess ethyl acetate
6. 6
   세척wash
7. 7
   건조dried over sodium sulfate
8. 8
   기타the solvent was removed under reduced pressure
9. 9
   기타The resulting crude product was used for the next step without further purification

실험 절차

H2SO4 (1.5 equiv.) was added to a suspension of LAH (3 equiv.) in THF (32 ml) at 0° C. and the mixture was stirred at room temperature for 0.5 h. A solution of 1-benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidine-4-carbonitrile (5.54 mmol, 1 equiv.) in THF was added under cooled conditions and the resulting reaction mixture was heated to 50° C. for 16 h. The reaction was quenched with THF/H2O solution, filtered and the solid residue washed with excess ethyl acetate. The organic layer was given a brine wash, dried over sodium sulfate and the solvent was removed under reduced pressure. The resulting crude product was used for the next step without further purification. Yield: 85%.

출처