反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
To a solution of methyl 5-methoxy-3-methylpyrazine-2-carboxylate (5.1 g, 28.0 mmol) in MeOH (50 mL) was added sodium hydroxide 1.0 N solution (30.8 mL, 30.8 mmol). The reaction was heated to 40° C. for 2 h. The reaction mixture was concentrated, diluted with water and pH adjusted to 4. The solid that precipitated was filtered and dried. The remaining acidic solution was extracted with EtOAc and DCM. The combined organics were dried with Na2SO4, and concentrated in vacuo to give another batch of solid. The solids were combined and dried to give 5-methoxy-3-methylpyrazine-2-carboxylic acid (4.5 g, 96% yield). 1H NMR (300 MHz, DMSO-d6) δ 13.00 (br. s., 1H), 8.18 (s, 1H), 3.96 (s, 3H), 2.67 (s, 3H).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additiondiluted with water
- customThe solid that precipitated
- filtrationwas filtered
- customdried
- extractionThe remaining acidic solution was extracted with EtOAc and DCM
- dry with materialThe combined organics were dried with Na2SO4
- concentrationconcentrated in vacuo
- customto give another batch of solid
- customdried