反应详情

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%.

1. customa small precipitation
2. filtrationwas filtered off
3. washwashed twice with 1 ml of DMF
4. customThe filtrates were collected
5. waitkept at room temperature overnight
6. addition50 ml of water was added to the solution
7. customA precipitated oil was separated by centrifugation
8. dissolutionThe residual oil was dissolved in 10 ml of methanol
9. addition0.2 ml of conc. HCl was added
10. concentrationThe methanol solution was concentrated to 2 ml
11. filtrationpurified by gel filtration on Sephadex