HRID479100

反应详情

EQUATION

反应方程式

HRID 479100 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 3-Chloromethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine 3 (70 mg; 0.33 mmol) and 1.0 mL of piperidine were heated to 80° C. in a sealed tube for 7 h. The mixture was then allowed to cool to room temperature and concentrated in vacuo. 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 111 mg of yellow colored 3-Piperidin-1-ylmethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine as the trifluoroacetate salt.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. concentrationconcentrated in vacuo
  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