HRID930458
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
In a 1-L flask, the methyl 3-methylpyrazine-2-carboxylate (step 1, 16.08 g, 106 mmol) was suspended in CHCl3 (300 mL). 3-chlorobenzoperoxoic acid (Aldrich, 24.62 g, 143 mmol) was added. The reaction mixture was heated to 70° C. for 16 h. The reaction mixture was quenched with saturated NaHCO3 (200 mL). The layers were separated, and the aqueous layer was further extracted with DCM (2×100 mL). The combined organic layers were dried over MgSO4, and the filtrate was concentrated to afford the title compound. MS m/z=169 [M+H]+. Calculated for C7H8N2O3: 168.
WORKUP
后处理
- customThe reaction mixture was quenched with saturated NaHCO3 (200 mL)
- customThe layers were separated
- extractionthe aqueous layer was further extracted with DCM (2×100 mL)
- dry with materialThe combined organic layers were dried over MgSO4
- concentrationthe filtrate was concentrated