HRID1830764

反应详情

EQUATION

反应方程式

HRID 1830764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a stirred solution of methanol (89 μL; 2.2 mmol) in dioxane (1 mL) was added sodium hydride (53 mg; 2.2 mmol). After stirring for 30 minutes, 2-amino-6-chloropyrazine (258 mg; 2.0 mmol) was added and the reaction was heated to 90° C. After stirring for 12 hours, the reaction was cooled to room temperature, diluted with 30 mL of ethyl acetate and washed with aqueous 10% sodium carbonate (1×30 mL), and brine (30 mL), then dried (MgSO4), and filtered. The crude product was purified using the Biotage 12i cartridge eluting with hexane and ethyl acetate (3:1) to yield a white solid (11% yield).

WORKUP

后处理

  1. stirringAfter stirring for 12 hours
  2. temperaturethe reaction was cooled to room temperature
  3. washwashed with aqueous 10% sodium carbonate (1×30 mL), and brine (30 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customThe crude product was purified
  7. washeluting with hexane and ethyl acetate (3:1)