HRID480449

反应详情

EQUATION

反应方程式

HRID 480449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-hydroxy-1-naphthaldehyde (60.0 g) in AcOH (300 mL) was added dropwise a solution of bromine (66.8 g) in AcOH (30 mL) over 30 min. After being stirred for 1 h, the mixture was poured into aqueous Na2S2O3 solution, and the resulting mixture was extracted with AcOEt. The combined organic layers were washed with water, 1N-NaOH, and brine followed by drying over MgSO4. After removal of the solvent in vacuo, the residue was washed with EtOH to give a yellow powder. The powder was crystallized from iPrOH to afford the title compound (28.8 g) as pale yellow needles.

WORKUP

后处理

  1. extractionthe resulting mixture was extracted with AcOEt
  2. washThe combined organic layers were washed with water, 1N-NaOH, and brine
  3. dry with materialby drying over MgSO4
  4. customAfter removal of the solvent in vacuo
  5. washthe residue was washed with EtOH
  6. customto give a yellow powder
  7. customThe powder was crystallized from iPrOH