Reacción #5825

Ecuación de reacción

dimethylformamide

homopiperazine

sodium bicarbonate

benzyloxycarbonyl chloride

→

title compound

Rendimiento 65.5%

N-Benzyloxycarbonylhomopiperazine

Rendimiento 65.5%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGthe mixture was stirred at a room temperature overnight
2. 2
   OtroAfter evaporating off dimethylformamide under a reduced pressure
3. 3
   Extracciónthe reaction mixture was extracted three times with 100 ml of chloroform
4. 4
   Secadothe extract was dried over magnesium sulfate
5. 5
   Otroevaporated
6. 6
   Otroto remove the solvent under a reduced pressure
7. 7
   Lavadoeluted with chloroform/methanol (9:1)

Procedimiento

To 230 ml of dimethylformamide were added 25 g of homopiperazine and 5.4 g of sodium bicarbonate and then 25 ml of water followed by dropwise addition of 10 g of benzyloxycarbonyl chloride with stirring under ice cooling, and the mixture was stirred at a room temperature overnight. After evaporating off dimethylformamide under a reduced pressure, the reaction mixture was extracted three times with 100 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (9:1), to obtain 9 g of the title compound as a light yellow liquor liquid.

Fuente