HRID1512190
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
A stirred mixture of 6-hydroxy-1-naphthalenecarboxylic acid, methyl ester (0.202 g, 1.0 mmol), 2-chloro-4-nitropyridine (0.174 mg, 1.1 mmol) and potassium carbonate (0.276 g, 2 mmol) in dimethylsulphoxide (5 mL) is heated at 70° C. for 1 h. The mixture is poured into water and the crude product is filtered off, washed with water. The crude product is dissolved in ethyl acetate, washed with brine, dried (Na2SO4) and the solvent is evaporated off under reduced pressure to give a residue which is recrystallized from ethylacetate-hexane to afford the title compound as a beige crystalline solid, m.p.: 103-104° C.
WORKUP
后处理
- filtrationthe crude product is filtered off
- washwashed with water
- dissolutionThe crude product is dissolved in ethyl acetate
- washwashed with brine
- dry with materialdried (Na2SO4)
- customthe solvent is evaporated off under reduced pressure
- customto give a residue which
- customis recrystallized from ethylacetate-hexane