반응 #71833

반응 방정식

ammonium formate

tert-butyl cis(±)-4-(benzylamino)-3-(benzyloxy)piperidine-1-carboxylate

tert-Butyl cis(±)-4-(benzylamino)-3-(benzyloxy)piperidine-1-carboxylate

→

crude title compound

수율 90.2%

tert-Butyl cis(±)-4-amino-3-(benzyloxy)piperidine-1-carboxylate

수율 90.2%

용매

methanol

반응 조건

후처리

1. 1
   여과The reaction solution was filtered
2. 2
   기타to remove the Pd/C
3. 3
   농축concentration under reduced pressure
4. 4
   workup.ADDITIONa 1 N aqueous sodium hydroxide solution was added to the residue
5. 5
   추출followed by extraction with dichloromethane three times
6. 6
   건조The organic layer was dried over anhydrous magnesium sulfate
7. 7
   농축concentrated under reduced pressure

실험 절차

10% Pd/C (wet, 1.1 g) and ammonium formate (2.87 g, 46 mmol) were added to a solution of tert-butyl cis(±)-4-(benzylamino)-3-(benzyloxy)piperidine-1-carboxylate obtained in Example (90c) (4.84 g, 11.4 mmol) in methanol (30 mL) in a nitrogen atmosphere, and the mixture was stirred at 70° C. for 40 minutes. The reaction solution was filtered to remove the Pd/C. Following concentration under reduced pressure, a 1 N aqueous sodium hydroxide solution was added to the residue, followed by extraction with dichloromethane three times. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure, to obtain 3.15 g of the crude title compound as a colorless oily substance (94%).

출처