HRID343367
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction was heated
- temperatureunder reflux for 18 hours
- customthe solvent removed by evaporation
- additionWater (5 ml) was added to the residue
- extractionextracted with dichloromethane (3×20 ml)
- dry with materialThe combined organic extracts were dried (MgSO4)
- customthe solvent removed by evaporation
- customThe residue was purified by chromatography on silica gel
- washeluting with dichloromethane