Reaktion #475961

Reaktionsgleichung

tert-Butyl piperidin-4-ylmethylcarbamate

Potassium carbonate

DIPEA

bromoacetonitrile

→

tert-butyl (1-(cyanomethyl)piperidin-4-yl)methylcarbamate

Lösungsmittel

CH3CN

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe solution was then concentrated
2. 2
   workup.ADDITIONsaturated NaHCO3 (40 mL) was added
3. 3
   ExtraktionThe mixture was extracted with CH2Cl2 (4×30 mL)
4. 4
   TrocknenThe extract was dried over anhydrous Na2SO4
5. 5
   ExtraktionThe dried extract
6. 6
   Waschenthe desired compound was eluted off with EtOAc
7. 7
   SonstigeThe product was further purified by crystallization from EtOAc/petroleum ether as a white solid (5.4 g, 92%)

Vorschrift

tert-Butyl piperidin-4-ylmethylcarbamate (5 g, 23.2 mmol) was dissolved in CH3CN (40 mL). Potassium carbonate (3.5 g, 25 mmol), DIPEA (4.4 mL, 25 mmol) and bromoacetonitrile (2.77 g, 23.2 mmol) were added, and the mixture was stirred at room temperature overnight. The solution was then concentrated and saturated NaHCO3 (40 mL) was added. The mixture was extracted with CH2Cl2 (4×30 mL). The extract was dried over anhydrous Na2SO4. The dried extract was passed through a silica gel plug, and the desired compound was eluted off with EtOAc. The product was further purified by crystallization from EtOAc/petroleum ether as a white solid (5.4 g, 92%).

Quelle