HRID1166787
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 cold (0° C.) suspension of 1-methylnaphthalene (5 g) in HNO3 was added H2SO4 (5 mL) dropwise. After stirring the reaction for one hour, the solution was diluted with ethyl acetate and washed with water (3×), aqueous saturated NaHCO3 (2×) and brine, dried over MgSO4, and concentrated. The product was purified by silica gel column chromatography using ethyl acetate:hexane (5:95) and recrystallized from methanol to give yellow needles.
WORKUP
后处理
- customthe reaction for one hour
- washwashed with water (3×), aqueous saturated NaHCO3 (2×) and brine
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe product was purified by silica gel column chromatography
- customrecrystallized from methanol
- customto give yellow needles