Reacción #1901066

Ecuación de reacción

1-methylpiperazine

1,3-di-p-tolylcarbodiimide

→

1-[(N,N′-Di-p-tolyl)amidino]-4-methyl-piperizine

Rendimiento 78.0%

Disolventes

N,N′-dimethylformamide

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroa small precipitation
2. 2
   Otrowas removed by filtration
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
   OtroAn oil precipitated after 0.5 h which
8. 8
   FiltraciónThe solid residue was collected by filtration
9. 9
   Lavadowashed twice with water
10. 10
    workup.DISSOLUTIONdissolved in 20 ml of methanol
11. 11
    workup.ADDITION0.2 ml of conc. HCl was added
12. 12
    workup.ADDITIONwas added to the methanol solution
13. 13
    OtroAfter evaporation of the methanol
14. 14
    workup.DISSOLUTIONthe residue was redissolved in methanol
15. 15
    Otropure product was precipitated from the solution with ethyl ether

Procedimiento

1.05 mmol of 1-methylpiperazine was dissolved in 10 ml of N,N′-dimethylformamide (DMF), and 1.0 mmol of 1,3-di-p-tolylcarbodiimide was added. After 0.5 h. of stirring at room temperature, a small precipitation was removed by filtration 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. An oil precipitated after 0.5 h which transformed into a solid. The solid residue was collected by filtration, washed twice with water and dissolved in 20 ml of methanol. 0.2 ml of conc. HCl was added was added to the methanol solution. After evaporation of the methanol, the residue was redissolved in methanol, and pure product was precipitated from the solution with ethyl ether. Yield=78%.

Fuente