反应详情

温度

100 °C

A mixture of 3-Chloromethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine 3 (2.00 g; 9.5 mmol) and piperazine (2.50 g; 29 mmol) in absolute ethanol was heated to 100° C. in a sealed tube for 4 h. The mixture was then allowed to cool to room temperature and evaporated. The crude product was purified by reverse phase HPLC (Rainin C18, 0% CH3CN to 30% CH3CN gradient, CH3CN/H2O, 0.1% TFA) and the bright yellow fractions containing the product were lyophilized after removal of CH3CN in vacuo to give 1.44 g of yellow colored 3-Piperazin-1-ylmethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine 5 as the trifluoroacetate salt.

1. temperatureto cool to room temperature
2. customevaporated
3. customThe crude product was purified by reverse phase HPLC (Rainin C18, 0% CH3CN to 30% CH3CN gradient, CH3CN/H2O, 0.1% TFA)
4. additionthe bright yellow fractions containing the product
5. customafter removal of CH3CN in vacuo