HRID1809645

反应详情

EQUATION

反应方程式

HRID 1809645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

3-(6-Chloro-3-methylpyridazin-4-yloxy)pyridin-2-amine (3.0 g, 12.7 mmol) was charged with MeOH (150 mL). Pd/C (0.67 g, 0.63 mmol) was added followed by ammonium formate (2.23 g, 35.5 mmol). The mixture was heated at 65° C. overnight. The solution was cooled and filtered through GF/F paper. The filtrate was concentrated and the residue was dissolved in dichloromethane and saturated NaHCO3. The organic layer was separated and the aqueous layer was extracted twice with dichloromethane. The combined organics were dried and concentrated to give 3-(3-methylpyridazin-4-yloxy)pyridin-2-amine (1.85 g, 72%) as a solid.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. filtrationfiltered through GF/F paper
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in dichloromethane
  5. customThe organic layer was separated
  6. extractionthe aqueous layer was extracted twice with dichloromethane
  7. customThe combined organics were dried
  8. concentrationconcentrated