Reacción #1901067

Ecuación de reacción

piperazine

1,3-di-p-tolylcarbodiimide

→

1-[(N,N′-Di-p-tolyl)amidino]piperizine

Rendimiento 52.0%

Disolventes

DMF

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroa small precipitation
2. 2
   Filtraciónwas filtered off
3. 3
   Lavadowashed twice with 1 ml of DMF
4. 4
   OtroThe filtrates were collected
5. 5
   workup.WAITkept at room temperature overnight
6. 6
   workup.ADDITION50 ml of water was added to the solution
7. 7
   OtroA precipitated oil was separated by centrifugation
8. 8
   workup.DISSOLUTIONThe residual oil was dissolved in 10 ml of methanol
9. 9
   workup.ADDITION0.2 ml of conc. HCl was added
10. 10
    ConcentraciónThe methanol solution was concentrated to 2 ml
11. 11
    Filtraciónpurified by gel filtration on Sephadex

Procedimiento

1.2 mmol of piperazine was dissolved in 10 ml of DMF and 1.0 mmol of 1,3-di-p-tolylcarbodiimide was added. After 0.5 hour of stirring at room temperature, a small precipitation was filtered off, and washed twice with 1 ml of DMF. The filtrates were collected and kept at room temperature overnight. 50 ml of water was added to the solution. A precipitated oil was separated by centrifugation. The residual oil was dissolved in 10 ml of methanol and 0.2 ml of conc. HCl was added. The methanol solution was concentrated to 2 ml and purified by gel filtration on Sephadex LH-20 in methanol. Yield=52%.

Fuente