HRID572493

反应详情

EQUATION

反应方程式

HRID 572493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of Hydroxyl-[7-hydroxy-2-methyl-4-(5-methyl-chroman-6-yl)-1-oxo-1,2-dihydro-isoquinolin-3-yl]-acetic acid methyl ester (600 mg, 1.465 mmol) in t-BuOAc (10 ml) was added HClO4 (512 mg, 5.12 mmol). The resultant mixture was stirred at RT under N2 for 2 h. The reaction mixture was diluted with water and extracted with EA (50 mL*3), dried over sodium sulfate and concentrated to dryness. The mixture was purified by chromatography column on silica gel to afford the title product (300 mg, 44%). LCMS (10-80 AB—2MIN.M): Rt=1.308, purity=96%, M+1=466.

WORKUP

后处理

  1. extractionextracted with EA (50 mL*3)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated to dryness
  4. customThe mixture was purified by chromatography column on silica gel