HRID911162

反应详情

EQUATION

反应方程式

HRID 911162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A high pressure steel bomb was charged with N-(4-(3-(2-fluoropyridin-4-yl)pyridin-4-yloxy)phenyl)-4-phenylphthalazin-1-amine (0.115 g, 0.237 mmol), potassium carbonate (0.049 g, 0.355 mol) and 3.0 mL of THF. The bomb was sealed, cooled to 0° C. and pressurized with methylamine gas. The reaction mixture was allowed to warm to RT, and heated at 80° C. for 45 h. Upon cooling, the reaction mixture was filtered through a fritted funnel, washed with MeOH, and concentrated. This mixture was purified by silica gel chromatography, (ISCO, 40 g column 0-10% MeOH/dichloromethane) to provide N-(4-(3-(2-(methylamino)pyridin-4-yl)pyridin-4-yloxy)phenyl)-4-phenylphthalazin-1-amine as a light yellow solid. MS m/z=497 [M+H]+. Calc'd for C31H24N6O: 496.56.

WORKUP

后处理

  1. customThe bomb was sealed
  2. temperatureto warm to RT
  3. temperatureheated at 80° C. for 45 h
  4. temperatureUpon cooling
  5. filtrationthe reaction mixture was filtered through a fritted funnel
  6. washwashed with MeOH
  7. concentrationconcentrated
  8. customThis mixture was purified by silica gel chromatography, (ISCO, 40 g column 0-10% MeOH/dichloromethane)