HRID2116493

反应详情

EQUATION

反应方程式

HRID 2116493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Next, a mixture of 4-(2-methoxymethoxyethyl)benzaldehyde (8.2 g, 42.1 mmol), methanol (160 mL), water (6 mL) and concentrated hydrochloric acid (4 mL) was stirred at 60° C. for 17.5 hours. After cooling to room temperature, the reaction mixture was neutralized with aqueous sodium hydroxide and evaporated under reduced pressure to remove methanol. The residue was extracted twice with ethyl acetate. The combined organic layers were washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. After concentration, the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10 to 50:50) to give 4-(2-hydroxyethyl)benzaldehyde (6.3 g).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. customevaporated under reduced pressure
  3. customto remove methanol
  4. extractionThe residue was extracted twice with ethyl acetate
  5. washThe combined organic layers were washed with saturated aqueous sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationAfter concentration
  8. customthe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10 to 50:50)