HRID1678744

反应详情

EQUATION

反应方程式

HRID 1678744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A suspension of 4-(3-methyl-9-phenyl[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl)benzaldehyde (13, 0.25 g, 0.69 mmol) and 2-amino-2,4-dimethylpentanoic acid (3-7, 0.101 g, 0.69 mmol) in DMF (3 mL) was heated at 150° C. for 30 min. The reaction mixture cooled and the solvent was removed in vacuo. The crude residue was dissolved in 3N HCl (2.5 mL) and was heated at 100° C. for 30 min. The mixture was cooled and purified via reverse phase HPLC (5-65% acetonitrile/water over 15 min) to give, upon evaporation of the solvents, the title compound as a yellow solid. HRMS m/z (M+1) Calcd: 366.1713. Found 366.1715.

WORKUP

后处理

  1. temperatureThe reaction mixture cooled
  2. customthe solvent was removed in vacuo
  3. dissolutionThe crude residue was dissolved in 3N HCl (2.5 mL)
  4. temperaturewas heated at 100° C. for 30 min
  5. temperatureThe mixture was cooled
  6. custompurified via reverse phase HPLC (5-65% acetonitrile/water over 15 min)
  7. customto give, upon evaporation of the solvents