Reaktion #74273

Reaktionsgleichung

LAH

1-benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidine-4-carbonitrile

H2SO4

→

desired product

Ausbeute 90.0%

(1-Benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidin-4-yl)methanamine

Ausbeute 90.0%

Lösungsmittel

THF

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturTo a cooled
2. 2
   Temperaturwas heated to 50° C. for 12 h
3. 3
   SonstigeThe mixture was quenched with sodium sulfate solution
4. 4
   Filtrationfiltered through celite
5. 5
   Waschenwashed with ethyl acetate
6. 6
   TrocknenThe organic layer was dried over sodium sulfate
7. 7
   Sonstigethe solvent was evaporated under reduced pressure

Vorschrift

To a cooled (0° C.) suspension of LAH (9.24 mmol, 3.0 equiv.) in THF (2 ml/mmol) was added dropwise conc. H2SO4 (4.62 mmol, 1.5 equiv.) in THF (1 ml/mmol) and the resulting suspension was stirred at room temperature for 1.5 h. A solution of 1-benzyl-4-(4-cyclopropylpiperazin-1-yl)piperidine-4-carbonitrile (3.08 mmol, 1.0 equiv.) in THF (2 ml/mmol) was added dropwise to the reaction mixture and it was heated to 50° C. for 12 h. The mixture was quenched with sodium sulfate solution, filtered through celite and washed with ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure to yield the desired product. Yield: 90%

Quelle