HRID1090854

反应详情

EQUATION

反应方程式

HRID 1090854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a hot (80° C.) solution of manganese(II) acetate tetrahydrate (858 mg, 3.50 mmol) in acetic acid (8 mL) were added sequentially potassium permanganate (138 mg, 0.875 mmol), acetic anhydride (1,355 mg, 10.5 mmol), anhydrous sodium acetate (420 mg, 5 mmol) and a solution of 2-benzoyl-1-[3,3-di(ethoxycarbonyl)propyl]pyrrole (500 mg, 1.40 mmol) in acetic acid (2 mL). The resulting mixture was stirred at 80° C. for 6 hours, cooled, poured into water (25 mL), and extracted with toluene (3×25 mL). The combined toluene extracts were washed with water (25 mL) and concentrated under reduced pressure to provide 478 mg (96%) of diethyl 5-benzoyl-2,3-dihydro-1H-pyrrolizine-1,1-dicarboxylate (I).

WORKUP

后处理

  1. temperaturecooled
  2. extractionextracted with toluene (3×25 mL)
  3. washThe combined toluene extracts were washed with water (25 mL)
  4. concentrationconcentrated under reduced pressure