HRID247795

反应详情

EQUATION

反应方程式

HRID 247795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

After a solution of decylmonobromide (7 g), 2-hydroxy-6-carboxynaphthalene (2 g) and anhydrous potassium carbonate (4 g) in dimethylformamide (100 ml) was stirred at 130° C. for two hours, it was poured in water. Dilute aqueous hydrochloric acid solution was added thereto until the solution was neutral. To the solution was added diethylether in order to effect extraction. The extracted layer was distilled to remove the solvent. The residue was added to a solution of sodium hydroxide (3.3 g) in water (10 ml) and ethanol (50 ml). The mixture was refluxed for about one day. Thereto was added dilute aqueous hydrochloric acid solution until the solution was neutral. The solution was distilled to remove the solvent and concentrated. Solid precipitate was collected and recrystallized from water-ethanol mixture to obtain the titled compound (2.4 g).

WORKUP

后处理

  1. extractionextraction
  2. distillationThe extracted layer was distilled
  3. customto remove the solvent
  4. additionThe residue was added to a solution of sodium hydroxide (3.3 g) in water (10 ml) and ethanol (50 ml)
  5. temperatureThe mixture was refluxed for about one day
  6. additionThereto was added dilute aqueous hydrochloric acid solution until the solution
  7. distillationThe solution was distilled
  8. customto remove the solvent
  9. concentrationconcentrated
  10. customSolid precipitate was collected
  11. customrecrystallized from water-ethanol mixture