HRID343367

反应详情

EQUATION

反应方程式

HRID 343367 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Amino-3-bromo-5-methylpyrazine (0.374 g) was added to a freshly prepared solution of sodium methoxide in methanol (made by addition of sodium (0.115 g) to methanol (6 ml)). The reaction was heated under reflux for 18 hours, cooled to ambient temperature and the solvent removed by evaporation. Water (5 ml) was added to the residue and extracted with dichloromethane (3×20 ml). The combined organic extracts were dried (MgSO4) and the solvent removed by evaporation. The residue was purified by chromatography on silica gel, eluting with dichloromethane to give 2-amino-3-methoxy-5-methylpyrazine as a white crystalline solid (0.208 g, 75%), m.p. 67°-69° C.; mass spectrum (+ve CI): 140 (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureunder reflux for 18 hours
  3. customthe solvent removed by evaporation
  4. additionWater (5 ml) was added to the residue
  5. extractionextracted with dichloromethane (3×20 ml)
  6. dry with materialThe combined organic extracts were dried (MgSO4)
  7. customthe solvent removed by evaporation
  8. customThe residue was purified by chromatography on silica gel
  9. washeluting with dichloromethane