Reaktion #2332390

Reaktionsgleichung

LAH

1,4-dibenzyl-piperazine-2-carboxylic acid amide

→

desired product

Ausbeute 99.0%

1,4-Dibenzyl-2-aminomethyl-piperazine

Ausbeute 99.0%

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 20 h (monitored by TLC)
2. 2
   TemperaturThe stirred mixture was cooled with an ice-bath
3. 3
   Sonstigequenched with Rochelle's salt (6 mL)
4. 4
   workup.ADDITIONthe suspension was poured over a pad of silica gel (20 mm)
5. 5
   WaschenThe celite was washed with 15% MeOH in CH2Cl2 with 1% NH4OH (3×50 mL)
6. 6
   Wascheneluted through pad of silica gel
7. 7
   EinengenTh eluent was concentrated under reduced pressure

Vorschrift

To a stirred suspension of LAH (0.9 g, 25.9 mmol) in dry THF (150 mL) was added 1,4-dibenzyl-piperazine-2-carboxylic acid amide (4.0 g, 12.93 mmol) and the mixture was stirred under reflux for 20 h (monitored by TLC). The stirred mixture was cooled with an ice-bath and quenched with Rochelle's salt (6 mL), warmed to room temperature, and the suspension was poured over a pad of silica gel (20 mm). The celite was washed with 15% MeOH in CH2Cl2 with 1% NH4OH (3×50 mL) and eluted through pad of silica gel. Th eluent was concentrated under reduced pressure to give the desired product in 99% yield.

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