HRID1056245
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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A glass microwave reaction vessel was charged with 5-chloro-2-methylpyrido[3,4-b]pyrazin-3-yl methanesulfonate (160 mg, 0.585 mmol), 1,4-Dioxane (1 mL) and hydrogen chloride (4 M in 1,4-dioxane, 0.73 mL, 2.92 mmol) (Sigma Aldich). The reaction mixture was stirred and heated in an oil bath at 70° C. for 1 h, then cooled to RT. The mixture was diluted with EtOAc (50 mL) and washed with sat. NaHCO3. The organic layer was dried (MgSO4), filtered and concentrated to give 3,5-dichloro-2-methylpyrido[3,4-b]pyrazine (62 mg, 0.290 mmol, 49% yield) as a brown solid. MS (ESI, pos. ion) m/z: 213.9 (M+1).
WORKUP
后处理
- customA glass microwave reaction vessel
- temperaturecooled to RT
- washwashed with sat. NaHCO3
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated