Reaktion #426886

Reaktionsgleichung

product

tert-butyl 4-(benzylamino)-3-fluoropiperidine-1-carboxylate

→

desired product

Ausbeute 97.4%

cis-tert-butyl 4-amino-3-fluoropiperidine-1-carboxylate

Ausbeute 97.4%

Lösungsmittel

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction was filtered through celite
2. 2
   Waschenthe celite was washed with EtOAc
3. 3
   EinengenThe filtrate was concentrated
4. 4
   workup.DISSOLUTIONthe residue was dissolved in CH2Cl2
5. 5
   Filtrationfiltered through celite
6. 6
   Waschenthe celite was washed with CH2Cl2 and EtOAc
7. 7
   EinengenThe filtrate was concentrated

Vorschrift

To a 250 mL glass Parr vessel was added the product from Step C (14.8 g, 48.0 mmol) and EtOH (100 mL). Pearlman's Catalyst (4.72 g, 3.36 mmol) was added and the mixture was shaken in a Parr reactor under 40-45 psi H2 for 15 hours. The reaction was filtered through celite and the celite was washed with EtOAc. The filtrate was concentrated and the residue was dissolved in CH2Cl2 and filtered through celite, and the celite was washed with CH2Cl2 and EtOAc. The filtrate was concentrated to afford 10.2 g (92%) of the desired product as a thick oil that slowly solidified to a white solid.

Quelle