HRID73496
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
- 50 °C
PROCEDURE
实验过程
Commercially available 6-Methyl-2-nitro-pyridin-3-ol (Aldrich) (5.09 g, 33 mmol) in acetone (50 mL) was treated with K2CO3 (5.47 g, 39.6 mmol) and MeI (3.09 mL, 49.5 mmol). The orange suspension was heated to 50° C. for 90 hours. After evaporation of the solvent in vacuo the crude mixture was treated with 1N NaOH (50 mL) and extracted with EtOAc (2×50 mL) the combined organic phases was washed with brine (2×50 mL), dried over Na2SO4, filtered and concentrated in vacuo. 3-Methoxy-6-methyl-2-nitro-pyridine was obtained as a yellow solid.
WORKUP
后处理
- customAfter evaporation of the solvent in vacuo the crude mixture
- additionwas treated with 1N NaOH (50 mL)
- extractionextracted with EtOAc (2×50 mL) the combined organic phases
- washwas washed with brine (2×50 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo