HRID1719276

反应详情

EQUATION

反应方程式

HRID 1719276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

Methyl 2-[(4R)-3-bromo-4-allyl-2-oxoazetidin-1-yl]-3-methyl-2-butenoate (840 mg) was dissolved in methylene chloride (6 ml) and cooled to 5° C. To this cooled solution were added acetic acid (0.5 ml) and zinc powder (0.60 g), and the mixture was allowed to warm to room temperature. After stirring for 30 minutes, the reaction mixture was diluted with ethyl acetate (6 ml) and filtered through a pad of Celite. The filtrate was further diluted with ethyl acetate (50 ml) and washed successively with water, dilute sodium bicarbonate and brine. Drying over magnesium sulfate and evaporation left an oil, which was chromatographed on silica gel (20 g) eluting with a mixture of benzene and acetone (5:1) to give methyl 2-[(4R)-4-allyl-2-oxoazetidin-1-yl]-3-methyl-2-butenoate (174 mg) as an oil.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. filtrationfiltered through a pad of Celite
  3. additionThe filtrate was further diluted with ethyl acetate (50 ml)
  4. washwashed successively with water, dilute sodium bicarbonate and brine
  5. dry with materialDrying over magnesium sulfate and evaporation
  6. waitleft an oil, which
  7. customwas chromatographed on silica gel (20 g)
  8. washeluting with a mixture of benzene and acetone (5:1)