HRID968003
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
To a mixture of 2-chloro-4-(1-ethyl-propoxy)-6-methyl-3-nitro-pyridin (500 mg, 1.93 mmol), and 2,4,6-trimethylphenol (289 mg, 2.13 mmol) in dry THF was added potassium t-butoxide. The resulting mixture was stirred at rt. overnight. The mixture was quenched with water, brine and extracted 3 times with ethyl acetate. The organic layer was separated, dried (MgSO4) and concentrated to dryness. After silica gel column chromatography purification, the title compound was obtained as a light yellow crystal, mp 106-109° C. Anal. For C20H26N2O4 calc. C, 67.02; H, 7.31; N, 7.82; found, C, 67.34; H, 7.40; N, 7.42.
WORKUP
后处理
- customovernight
- customThe mixture was quenched with water, brine
- extractionextracted 3 times with ethyl acetate
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- concentrationconcentrated to dryness
- customAfter silica gel column chromatography purification