HRID1913831

反应详情

EQUATION

反应方程式

HRID 1913831 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 6-methoxyisochromen-1-one (9.3 g) in dichloromethane (300 ml) was added, at 0° C., a solution of boron tribromide (1 M in dichloromethane, 130 ml), and the mixture was stirred at room temperature for 16 hours. After sodium carbonate solution had been added, the mixture was washed with ethyl acetate. The aqueous phase was acidified with 2 N HCl and extracted with ethyl acetate. The organic phases were dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel. The product was thus obtained with the molecular weight of 162.15 (C9H6O3); MS (ESI): 163 (M+H+).

WORKUP

后处理

  1. washthe mixture was washed with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phases were dried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel
  6. customThe product was thus obtained with the molecular weight of 162.15 (C9H6O3)