HRID1512190

反应详情

EQUATION

反应方程式

HRID 1512190 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationthe crude product is filtered off
  2. washwashed with water
  3. dissolutionThe crude product is dissolved in ethyl acetate
  4. washwashed with brine
  5. dry with materialdried (Na2SO4)
  6. customthe solvent is evaporated off under reduced pressure
  7. customto give a residue which
  8. customis recrystallized from ethylacetate-hexane