HRID2413372

反应详情

EQUATION

反应方程式

HRID 2413372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

653 mg (1.8 mmols) of (-)-1-(6-methoxy-2-naphthyl)-2-(ethoxycarbonyl)amino-1-propanone dimethyl acetal and 5 ml of a 30% aqueous potassium hydroxide solution were heated at reflux in 50 ml of methanol for 5 days. After adding 20 ml of water, the mixture was extracted with ethyl acetate (20 ml×3), and the extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (Florisil, ethyl acetate) to obtain 300 mg of (+)-1-(6-methoxy-2-naphthyl)-2-amino-1-propanone dimethyl acetal as colorless crystals having a melting point of 84°-86° C. Yield, 58%.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate (20 ml×3)
  2. dry with materialthe extract was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography (Florisil, ethyl acetate)