HRID1830774

反应详情

EQUATION

反应方程式

HRID 1830774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirred solution of 2-chloro-3,5-dimethyl pyrazine (1.0 mL; 8.3 mmol) in dimethylformamide (10 ml,) was added sodium azide (539 mg; 8.3 mmol). The reaction was heated to 100° C. and stirred for 12 hours. The reaction was cooled to room temperature, diluted with 50 mL of ethyl acetate and washed with aqueous 10% sodium carbonate (1×50 mL), brine (50 mL), then dried (MgSO4), and filtered. The material was purified using a biotage 12L cartridge eluting with hexanes and ethyl acetate (3: 1) to yield an off white solid (42% yield).

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. washwashed with aqueous 10% sodium carbonate (1×50 mL), brine (50 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customThe material was purified
  6. washeluting with hexanes and ethyl acetate (3: 1)